Month: March 2021

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 2905-67-1 as follows. Computed Properties of C8H6Cl2O2

Methyl 3,5-dichlorobenzoate (2-D) (1.07 g, 5.0 mmol) was suspended in a vigorously stirring solution of methylamine (40%/H20, 5.0 mL). After heating gently for 10 min, the mixture was stirred at room temperature for 18 h. The mixture was extracted with methylene chloride and the extract dried (MgS04) to provide 3,5-dichloro-N-methylbenzamide (2-E).

According to the analysis of related databases, 2905-67-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; MERCK & CO., INC.; WO2005/97759; (2005); A1;,
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Electric Literature of 57486-67-6, A common heterocyclic compound, 57486-67-6, name is Methyl 2-(2-fluorophenyl)acetate, molecular formula is C9H9FO2, its 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.

1-tert-butyl 4-methyl 4-(2-fluorophenyl)piperidine-1,4-dicarboxylate. A flask was charged with sodium hydride (2.14 g, 89.2 mmol) and dimethylformamide (70 ml) at 0 C. under nitrogen. Methyl 2-(2-fluorophenyl)acetate (5 g, 29.7 mmol) was added to the flask, and after stirring for 25 min, tert-butyl bis(2-chloroethyl)carbamate (8.6 g, 35.6 mmol) was added. The reaction was allowed to warm to rt and stirred overnight. The reaction was quenched with a saturated solution of ammonium chloride and extracted with ethyl acetate (5¡Á100 mL). The organics were collected, washed with brine, dried over sodium sulfate, and concentrated in vacuo. The residue was purified via silica gel chromatography (10/90?50/50 ethyl acetate/hexanes) to yield 1.7 g (17%) of the desired product. 1H-NMR (CDCl3, 400 MHz) delta ppm 7.29 (m, 1H), 7.24 (m, 1H), 7.12 (m, 1H), 7.00 (m, 1H), 3.86 (m, 2H), 3.67 (m, 3H), 3.22 (m, 2H), 2.37 (m, 2H), 1.96 (m, 2H), 1.44 (s, 9H). Mass spec.: 360.22 (MNa)+. LC tr=3.503 min (Phenomenex-Luna 4.6¡Á50 mm S10, 10% MeOH/90% H2O/0.1% TFA?90% MeOH/10% H2O/0.1% TFA Gradient Time=4 min, Flow rate=4 mL/min)

The synthetic route of 57486-67-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Squibb Company; US2007/249607; (2007); A1;,
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Electric Literature of 17994-94-4, The chemical industry reduces the impact on the environment during synthesis 17994-94-4, name is Methyl 7-aminoheptanoate hydrochloride, I believe this compound will play a more active role in future production and life.

Methyl 7-(4-(l^-dioxo-l,3-bis(quinolin-8-ylamino)pr pan-2-yl)benzamido)heptanoate, 60.; To compound 59 (200 mg, 0.42 mmol) in (?(? (20 mL) at rt added 7-aminoheptanoic acid methyl ester (as the hydrochloride, 90 mg, 0.46 mmol), Et^ (47 mg, 0.46 mmol) and EDC (89 mg, 0.46 mmol). The mixture was allowed to stir at rt for 12 h. Water was added and the mixture was worked up with Combined organic extracts were dried with anhydNa2S04, solvent removed under vacuum and the residue was purified by column chromatography (silica gel 230-400 mesh, 80% ethyl acetate in hexanes as the eluent) to afford 70 as a white solid (202 mg, 78%).Mp = 178-180 C. NMR (300 MHz, CDC13): delta = 1.34-1.36 (m, 4 H), 1.59-1.62 (m, 4 H), 2.29 (t, 2 H, J = 5.7 Hz), 3.42 (m, 2 H), 3.64 (s, 3 H), 5.03 (s, 1 H), 6.14 (s, 1 H), 7.43-7.47 (m, 2 H), 7.53 (d, 4 H, J = 3.3 Hz), 7.84 (dd, 4 H, /, = 6.3 Hz, J2 = 15.3 Hz), 8.15 (d, 2 H, J = 6 Hz), 8.82-8.86 (m, 4 H), 10.98 (s, 2 H). I3C NMR (75 MHz, CDC13): delta = 24.7, 26.5, 28.7, 29.4, 33.9, 40.0, 51.5, 62.3, 117.1, 121.7, 122.4, 127.1, 127.9, 128.7, 134.1, 134.8, 136.2, 138.0, 138.7, 148.7, 166.6, 167.0, 174.2. HRMS (FAB+) Calcd for C36H36O5N5 = 618.2638, Found = 618.2712.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 7-aminoheptanoate hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH; BRESLOW, Ronald; MARKS, Paul, A.; ABHILASH, K., G.; WANG, Jianing; WO2011/146855; (2011); A1;,
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Electric Literature of 52449-43-1, 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. 52449-43-1, name is Methyl 4-chlorophenylacetate, This compound has unique chemical properties. The synthetic route is as follows.

Referential Example 2 Methyl (4-chlorophenyl)bromoacetate To a solution of 102 g (0.55 mole) of methyl (4-chlorophenyl)acetate in 100 ml of carbon tetrachloride was added 97.9 g (0.55 mole) of N-bromosuccinimide. The resulting mixture was refluxed and irradiated with a 500 W bromo lamp for 5 hours. It was then cooled, filtered, and the filtrate was evaporated to dryness to give 150 g (103% yield) of methyl (4-chlorophenyl)bromoacetate. NMR (CDCl3) delta ppm; 3.79 (3H, s), 5,31 (1H, s), 7.3-7.7 (4H, s)

The chemical industry reduces the impact on the environment during synthesis Methyl 4-chlorophenylacetate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SUMITOMO PHARMACEUTICALS COMPANY, LIMITED; SUMITOMO CHEMICAL COMPANY, LIMITED; EP256687; (1991); B1;,
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These common heterocyclic compound, 2178-24-7, name is Ethyl (2-bromophenyl)acetate, its 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: 2178-24-7

EXAMPLE 35 alpha-{3-Amino-4-chloro-6-[N-(2-[diethylamino]ethyl)]carbamoylphenoxy}phenylacetic acid, ethyl ester To a well-stirred suspension of sodium hydride (0.36 g of 60%, 9 mmoles, washed with n-pentane) in 5 ml of dry DMF was added a solution of 4-amino-5-chloro-N-[2-(diethylamino)ethyl]2-hydroxybenzamide (2.28 g, 8 mmoles) (from Preparation No. 1B) in 10 ml of dry DMF. After evolution of hydrogen had ceased, to this was added dropwise a solution of ethyl alpha-bromophenyl acetate (2.12 g, 8.7 mmoles) in 5 ml of dry DMF. After an additional 18 hours at ambient temperature, the mixture was concentrated in vacuo and the residue partitioned between water (200 ml) and methylene chloride (75 ml). The aqueous phase was extracted twice with 75 ml portions of methylene chloride. After combining, the organic phase was washed three times with 50 ml of 10% aqueous sodium hydroxide and three times with brine; dried over sodium sulfate, filtered, concentrated in vacuo, to give 3.5 g of oil which slowly crystallized. Trituration with pentane gave 3.34 g of the title compound, mp. 84-87 C. The NMR spectrum (90 MHz) in CDCl3 gave the following resonances: delta8.55 (bt, 1H); 8.20 (s, 1H); 7.50 (m, 5H); 6.09 (s, 1H); 5.65 (s, 1H); 4.25 (m, 4H); 3.55 (m, 2H); 2.60 (m, 6H); 1.05 (m, 9H). Anal. Calc’d. for C23 H30 ClN3 O4: C, 61.66; H, 6.76; N, 9.38. Found: C, 61.75; H, 6.76; N, 9.27.

The synthetic route of Ethyl (2-bromophenyl)acetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bristol-Myers Company; US4808624; (1989); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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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Ester – an overview | ScienceDirect Topics

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;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics