Hydroxymethyl-7-Aminocephalosporanic acid synthesis

Yield:15690-38-7 90.1%

Reaction Conditions:

with tetrabutyl-ammonium chloride;sodium hydroxide in methanol;water at -5 - 5;

Steps:

1 Synthesis of 7-Amino-3-Hydroxymethylcephalosporanic Acid (7-DACA, Compound 6)
Weigh 7-ACA 27.2g (0.1mol),Add 50mL of methanol and 50mL of water,Add 3.0g tetra-n-butane at -5-5°CAmmonium chloride stirring to dissolve,Maintain the addition of 2mol/L sodium hydroxide solution 105mL at this temperature.After dripping, maintain the temperature and continue stirring for 0.5-1 hour.Then add 30% hydrochloric acid to adjust the pH to neutral,Precipitation of solids, suction filtration, anhydrous ethanol washing,20.7g of dried white solidYield 90.1%,HPLC purity analysis 97.35% (area normalization method),Lactone impurity 0.33%.

References:

Shandong Luoxin Pharmaceutical Group Co., Ltd.;Wang Jinxing;Hou Xiaolong;Xu Qinyan CN105131017, 2017, B Location in patent:Paragraph 0041-0042

FullText