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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 3196-23-4, name is Methyl 1-bromocyclohexanecarboxylate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 1-bromocyclohexanecarboxylate

General procedure: Synthesis. The mixture of zinc (3.0 g, 46 mmol), methyl 1-bromocycloalkanecarboxylate (12 mmol), HgCl2 (5 mg), and N,N-bis(arylmethylidene)benzidine 3 (5 mmol) in dry toluene(20 mL) with 2mL of HMPA was heated for 4 h under reflux and then cooled down, decanted from the zinc excess, and treated with 5% acetic acid. Organic layer was separated, and the aqueous layer was twice extracted with ethyl acetate. The combined organic layers were dried over Na2SO4 and then concentrated. The residue was purified by the recrystallization from p-xylene to give the reaction products 6a-i and 7a-k as white or Slightly colored Solids.

The synthetic route of 3196-23-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kirillov; Nikiforova; Baibarodskikh; Zakharova; Govorushkin; Journal of Chemistry; vol. 2019; (2019);,
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Electric Literature of 28170-07-2, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 28170-07-2, name is Benzyl phenyl carbonate, This compound has unique chemical properties. The synthetic route is as follows.

According to: Pittelkow, M.; Lewinsky, R.; and Christensen, J. B. Synthesis 2002, 15, 2195-2202.Benzyl phenylcarbonate (25,1 g, 1 10 mmol) was added dropwise to a solution of diethylenetriamine (5,16 g, 50 mmol) in dichloromethane (100 ml). The mixture was stirred for at least 20 h. The organic phase was washed with phosphate buffer (0.025 M K2HPO4,0.025 M NaH2PO4, 2000 ml, pH adjusted to 3 with 2 M sulfuric acid). The organic phase was dried over sodium sulfate, filtered, and concentrated in vacuo.Yield: 25.2 g A portion (5 g) of the crude oil was mixed with hydrochloric acid (2 M, 15 ml). The mixture was stirred for 15 minutes. The mixture was filtered. The isolated solid was mixed with abs. ethanol (600 ml). The mixture was brought to reflux. The boiling mixture was decanted in order to remove insoluble impurities. The compound crystallized over night at 5 C.Yield: 2.84 g (white crystals) 1H-NMR (af-DMSO) delta: 8.96 (b, 2H), 7.51 (t, J = 5.56 Hz, 2H), 7.40-7.30 (b, 10H), 5,04 (s,4H), 3.33 (q, J = 6.06 Hz, 4H), 3.00 (b, 4H)13C- NMR (Gf-DMSO) delta: 156.6, 137.2, 128.7, 128.3, 128.2, 66.0, 46.8, 37.1LC-MS (ES-positive mode), m/z: 372.5 [M+H]+

The chemical industry reduces the impact on the environment during synthesis Benzyl phenyl carbonate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; NOVO NORDISK A/S; WO2006/87354; (2006); A2;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 17994-94-4 as follows. Recommanded Product: 17994-94-4

General procedure: To a mixture of aldehyde (1 mmol) and amine/amine hydrochloride (1 mmol) in anhydrous CH2Cl2 (10 mL) was added triethylamine (2.5 mmol) at rt, and the resulting solution was stirred vigorously for 1 h. To this was then added (Boc)2O (1.2 mmol) followed by sodium triacetoxyborohydride (2 mmol). The reaction was stirred for an additional 4 h at rt, quenched with saturated NaHCO3 solution, and extracted with CH2Cl2. The combined organic fractions were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. The crude residue was purified by flash chromatography (95:05?50:50, hexanes/EtOAc) to afford the N-Boc secondary amine. Most of the title compounds were present as a mixture of rotational isomers in their 1H and 13C NMR spectra.

According to the analysis of related databases, 17994-94-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Neelarapu, Raghupathi; Petukhov, Pavel A.; Tetrahedron; vol. 68; 35; (2012); p. 7056 – 7062;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 609-12-1, name is Ethyl 2-bromo-3-methylbutanoate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H13BrO2

A mixture of 4-hydroxy-2-methylindole (1) (1.5 g, 0.010 mole), 2-bromo-3-methyl-butyric acid ethyl ester (2.2 g, 0.010 mole) and potassium carbonate (excess) in acetone (50 mL) was refluxed for 3 days. The reaction mixture was filtered, and the filtrate was concentrated. The residue was purified by column chromatography (20:1 Hex:EtOAc) to afford intermediate 2. Yield: 1.88 g, 71%

According to the analysis of related databases, 609-12-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Chang, Han-Ting; Charmot, Dominique; Glinka, Tomasz; Cope, Michael James; Goka, Elizabeth; Shao, Jun; Cartigny, Damien; Chen, Shiah-yun; Buysse, Jerry M.; US2007/135385; (2007); A1;,
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Application of 431-47-0, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 431-47-0 name is Methyl 2,2,2-trifluoroacetate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

e) 2,2,2-Trifluoro-N-prop-2-ynyl-acetamide To 15 g (272.3 mmol) propargylamine in 275 ml anhydrous methanol 36.6 g (285.9 mmol) methyl trifluoroacetate were added with cooling. The resulting reaction mixture was stirred for an additional four hours at room temperature. Afterwards the solvent was removed by distillation at reduced pressure. The residue was dissolved in 300 ml trichloromethane and extracted four times, twice each with 300 ml of a saturated sodium bicarbonate solution and twice each with 300 ml water. The separated organic phase was dried over magnesium sulfate, filtrated and the solvent was removed by distillation (yield: 23.3 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2,2,2-trifluoroacetate, and friends who are interested can also refer to it.

Reference:
Patent; Roche Diagnostics GmbH; F.HOFFMANN-LA ROCHE AG; EP1842923; (2007); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 5048-82-8, name is Ethyl 3-(4-aminophenyl)acrylate, A new synthetic method of this compound is introduced below., HPLC of Formula: C11H13NO2

PREPARATION 44 To a mixture of ethyl 4-aminocinnamate (300 mg), triethylamine (167 mg) and dichloromethane (3 ml) was added a solution of propionyl chloride (182 mg) in dichloromethane (1 ml) in an ice-water bath, and the mixture was stirred for 1 hour at the same temperature. To the reaction mixture was added 4 drops of N,N-dimethylpropanediamine, and the mixture was further stirred for 5 minutes. The reaction mixture was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was crystallized from diisopropyl ether to give ethyl 4-propionamidocinnamate (341 mg) as a colorless powder. mp: 138¡ã C. NMR (CDCl3, delta): 1.26 (3H, t, J=8 Hz), 1.34 (3H, t, J=8 Hz), 2.42 (2H, q, J=8 Hz), 4.26 (2H, q, J=8 Hz), 6.37 (1H, d, J=16 Hz), 7.21 (1H, br s), 7.49 (2H, d, J=8 Hz), 7.58 (2H, d, J=8 Hz), 7.68 (1H, d, J=16 Hz)

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd; US5574042; (1996); A;,
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Application of 555-43-1,Some common heterocyclic compound, 555-43-1, name is Propane-1,2,3-triyl tristearate, molecular formula is C57H110O6, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Alcoholysis of triglycerides Alcoholysis of pure triglycerides (TGs), including trilaurin, tripalmitin and tristearin, was carried out. Most diglyceride (DG) obtained from alcoholysis reaction were 1,2-DG. A high amount OF uNREACTED TG remained in the reaction mixture. Acyl migration was observed during the reaction, especially in hydrolysis reaction, as illustrated in Figure 18. Figure 18 shows data from alcoholysis reaction showing the 1,3- DS/1, 2-DS ratio during alcoholysis and hydrolysis of tristearin. DEP = D-EP100, RM = Lipozyme RM IM, Hx = n-hexane, HYD = hydrolysis, ALC = alcoholysis. The reaction catalyzed by Lipozyme RM IMTM, though gave lower yield, showed higher acyl migration than the reaction catalyzed by D-EP100. Low acyl migration was observed in alcoholysis using CAL-B after 6h. This could be because 1,2- DG and 1,3-DG were produced at the same time according to the non-specificity of CAL- B. D-EP 100 showed higher activity than CAL-B and Lipozyme RM, respectively, in alcoholysis of tripalmitin and tristearin. Effect OF AW : HIGHER yield and less MG was obtained from alcoholysis at aW 0.11 than 0.43. It was found that MG was increased with increasing aw. Effect of solvents (on yield and acyl migration): Highest yield was obtained with MTBE. Alcoholysis in n-hexane and isooctane gave moderate yield, while acetone was a poor solvent for Lipozyme RM. The reaction performed in n- hexane showed faster acyl migration than in MTBE, as illustrated in Figures 18 and 19. Figure 19 illustrates data from the hydrolysis of trilaurin at 60C by Lipozyme RM IM (DG = dilaurin).

The synthetic route of 555-43-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; DIVERSA CORPORATION; WO2005/32496; (2005); A2;,
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Synthetic Route of 1132-95-2,Some common heterocyclic compound, 1132-95-2, name is 1,1-Diisopropoxycyclohexane, molecular formula is C12H24O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The product from (1) was dissolved in 310 mL of acetone. 127,5 g of 1,1- diisopropoxycyclohexane and 31.0 g of pyridine hydrobromide were added. The mixture was stirred at 40-45 C for 3 hours. Then 300 mL of isopropyl acetate, 250 mL of 5% aqueous sodium carbonate and 9 mL of 20% aqueous sodium hydroxide were added. After stirring the aqueous phase was seperated off, and the organic phase was concentrated by distilling under vacuum. 246 g of a mixture 2′, 4″-0- bis (trimethylsilyl) erythromycin A 9- {O- [1- (1- methylethoxy)-cyclohexyl] oxime} and isopropyl acetate was obtained.; (2) The product obtained above in (1) was dissolved in 310 mL of acetone. 127,5 g of 1,1- diisopropoxycyclohexane and 31.0 g of pyridine hydrobromide were then added. The mixture was stirred at 40-45 C for 3 hours. Then 300 mL of isopropyl acetate, 250 mL of 5% aqueous sodium carbonate and 9 mL of 20% aqueous sodium hydroxide were added. After stirring and the aqueous phase was seperated off, and the organic phase was concentrated by distilling under vacuum. 236 g of a mixture 2′, 4″-0- bis (trimethylsilyl) erythromycin A 9- {O- [1- (1-methylethoxy)-cyclohexyl] oxime} and isopropyl acetate was obtained.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1-Diisopropoxycyclohexane, its application will become more common.

Reference:
Patent; SANDOZ AG; WO2005/90377; (2005); A1;,
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Application of 27492-84-8, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 27492-84-8 as follows.

General procedure: To a suspension of 5,6,6a,7,8,9-hexahydro-4H-phenalene-2-carboxylic acid (0.338 g, 1.56 mmol) in benzene (7.5 ml) was added SOCl2 (2.5 ml). The reaction mixture was refluxed for 4 h, then evaporated, and the residue was dissolved in benzene (3 ml) and pyridine (10 ml). Methyl 4-aminobenzoate (0.259 g, 1.71 mmol) and 4-DMAP (0.020 g, 0.164 mmol) were added to the resulting solution. The reaction mixture was stirred at rt for 15 h, then poured into 2 M aqueous HCl and extracted with AcOEt. The organic phase was washed with 10percent aqueous Na2CO3. Usual work-up gave a residue, which was purified by silica gel column chromatography(AcOEt/n-hexane = 1:10) to afford methyl 4-[(5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)carboxamido]benzoate (0.478 g,88percent). To a suspension of the above ester (0.385 g, 1.10 mmol) in EtOH (10 ml) was added 2 M aqueous NaOH (7.5 ml). The reaction mixture was stirred at 60 ¡ãC for 1 h, then cooled, acidified by adding 2 M aqueous HCl and extracted with CHCl3. Usual work-up gave a residue, which was purified by recrystallization from EtOH to afford 7a (0.348 g, 94percent).

According to the analysis of related databases, 27492-84-8, the application of this compound in the production field has become more and more popular.

Reference:
Article; Amano, Yohei; Noguchi, Masayuki; Nakagomi, Madoka; Muratake, Hideaki; Fukasawa, Hiroshi; Shudo, Koichi; Bioorganic and Medicinal Chemistry; vol. 21; 14; (2013); p. 4342 – 4350;,
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Some common heterocyclic compound, 924-99-2, name is Ethyl 3-(dimethylamino)acrylate, molecular formula is C7H13NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 924-99-2

b) Ethyl 3-dimethylamino-2-(2-fluoro-4acetoxybenzoyl)-2-propenoateA stirred solution of Intermediate 25a (4.91 g) in DCM (80 mL) at 200C was treated with oxalyl chloride (3.25 mL) and DMF (2 drops). After 2 h the clear solution was evaporated and re-evaporated from DCM (2x). The acid chloride was re-dissolved in toluene (100 mL) and treated with triethylamine (5.17 mL) and ethyl 3-dimethylaminopropenoate (4.13 g). After stirring for 2 h at 900C the mixture was filtered and the solution flash chromatographed (silica gel 40 to 100% EtOAc in petroleum ether [b.p. 40-600C]) to give the title compound as a yellow gum (4.3 g); APCI m/z 324.0 [M+H]+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 924-99-2, its application will become more common.

Reference:
Patent; GLAXO GROUP LIMITED; WO2006/50940; (2006); A1;,
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