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ChemicalBook CAS DataBase List 7-AVCA
79349-82-9

7-AVCA synthesis

4synthesis methods
33748-00-4 Synthesis
Cefixime Impurity

33748-00-4
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Yield:79349-82-9 93.8%

Reaction Conditions:

with acetic acid in phenol at 35; for 6 h;Temperature;Reagent/catalyst;

Steps:

3.4 Preparation of AVNA
GVNA25.5g (0.05 mol) was put into a 1,000 mL three-necked flask equipped with a thermometer and mechanical stirring, 300 g of phenol was added, 2.8 g of acetic acid was added and incubated at 35C After the reaction was completed for 6 hours, the reaction mixture was gradually poured into a mixed solution of baking soda (sodium hydrogencarbonate), purified water and butyl acetate (5 g of purified water, 200 ml of purified water and 200 ml of butyl acetate) The water layer was extracted twice with 50 mL of butyl acetate and the aqueous layer was again collected. The aqueous layer was put into a 500-ml reaction flask, and the reaction mixture was poured into a reaction vessel. The reaction mixture was stirred at room temperature for 2 hours, After adding 4 g of immobilized acylase PGA-450, 15% sodium carbonate aqueous solution was added dropwise to control the pH value of 8.0-8.2. The GVNA was <0.5% by HPLC. The enzyme was recovered by filtration. The filtrate was collected and adjusted to pH 3.4 with 10% The filter cake was rinsed with 50 ml of acetone and dried to give 10.7 g of AVNA (yield of AVNA 93.8%, calculated as GVNA).

References:

Shandong Apeloa Pharmaceutical Co., Ltd;Li, Kun;Meng, Jie;Wu, Zhongwen;Wei, Wei;Ge, Zhengliang;Ren, Hongyang;Zhou, Guoying CN104045655, 2016, B Location in patent:Paragraph 0061

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