반응 #1365530

반응 방정식

phosphorus pentachloride

p-methoxybenzyl 7-phenoxyacetamido-3-methylenecepham-4-carboxylate

methylene chloride

pyridine

→

p-Methoxybenzyl 7-amino-3-methylenecepham-4-carboxylate hydrochloride

용매

isobutanol

반응 조건

후처리

1. 1
   온도The reaction mixture was then cooled in an ice-water bath
2. 2
   기타of the reaction product, p-methoxybenzyl 7-amino-3-methylenecepham-4-carboxylate hydrochloride, precipitated from the mixture
3. 3
   여과The product was filtered
4. 4
   세척washed with cold methylene chloride
5. 5
   기타was dried in vacuo

실험 절차

To a solution of 4.3 g. of p-methoxybenzyl 7-phenoxyacetamido-3-methylenecepham-4-carboxylate in 50 ml. of methylene chloride were added 880 mg. of dry pyridine and 2.3 g. of phosphorus pentachloride and the mixture was stirred at the reflux temperature for 3 hours. The reaction mixture was then cooled in an ice-water bath and 5 ml. of isobutanol were added. The mixture was stirred in the cold for several hours during which time 2.2 g. of the reaction product, p-methoxybenzyl 7-amino-3-methylenecepham-4-carboxylate hydrochloride, precipitated from the mixture. The product was filtered and washed with cold methylene chloride and was dried in vacuo.

출처