New downstream synthetic route of 5335-05-7

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

Adding a certain compound to certain chemical reactions, such as: 5335-05-7, name is Chloromethyl benzoate, belongs to esters-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 5335-05-7, Recommanded Product: Chloromethyl benzoate

A solution of [2- (8, 9-DIOXO-2, 6-DIAZABICYCLO [5.2. 0] non-1 (7)-en-2-yl) ethyl]- phosphonic acid (20.16 MMOL, 5.25 g) in dry DMF (120 mL) was treated with N, N- diisopropylethylamine (80.64 MMOL, 14 ml) for’/2 hour at ambient temperature. Benzoic acid chloromethyl ester (60.49 MMOL, 10.32 g, synthesis described below) was added at ambient temperature under exclusion of moisture. The reaction mixture was heated to 65C for 20 hours. The temperature was then raised to 72C and stirred at 72C for 16 hours after which the reaction was completed. The mixture was cooled to room temperature and partitioned between 10% sodium bicarbonate and ethyl acetate. After separation of the layers the aqueous phase was again extracted with ethyl acetate (6x) until there was no more product in the water phase (by silica gel TLC, 7% 2M ammonia in methanol and 93% chloroform). The combined organic layers were washed with brine, dried over magnesium sulfate, filtered and evaporated to dryness. The residue was flash chromatographed on 400 g silica gel using a solvent mixture of 1 % 2M ammonia in methanol and 99% chloroform. Gradually the percentage of ammonia in methanol was increased to 7% and 93% chloroform. The solvent was evaporated in vacuo to yield the desired product (10.5 g, 99%; glass like material). MS (ES-): m/e 527 (M-H).

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

Reference:
Patent; WYETH; WO2004/92189; (2004); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics