반응 #93024

반응 방정식

benzhydryl 7-phenylacetamido-3-formyl-2-cephem-4-carboxylate

triphenylphosphine

carbon tetrachloride

ethyl acetate

→

benzhydryl 7-phenylacetamido-3-(2,2-dichlorovinyl)-2-cephem-4-carboxylate

용매

N,N-dimethylacetamide

반응 조건

후처리

1. 1
   온도After being cooled
2. 2
   기타the resulting precipitates
3. 3
   여과were filtered off
4. 4
   기타the filtrate was evaporated in vacuo
5. 5
   기타The residue was purified by column chromatography on silica gel

실험 절차

Zinc powder (78.4 g) was added to a solution of benzhydryl 7-phenylacetamido-3-formyl-2-cephem-4-carboxylate (102.4 g) and triphenylphosphine (367.2 g) in a mixture of carbon tetrachloride (800 ml) and N,N-dimethylacetamide (200 ml) at ambient temperature and the mixture was stirred at 60° C. for 30 minutes. After being cooled, the mixture was added to ethyl acetate (20 l) and the resulting precipitates were filtered off and the filtrate was evaporated in vacuo. The residue was purified by column chromatography on silica gel to give benzhydryl 7-phenylacetamido-3-(2,2-dichlorovinyl)-2-cephem-4-carboxylate (15.26 g).

출처