反応 #94845

反応方程式

methanol

benzyl 7β-(2-phenoxyacetamido)-2-oxo-3-cephem-4-carboxylate

N,N-dimethylaniline

phosphorus pentachloride

→

benzyl 7βamino-2-oxo-3-cephem-4-carboxylate hydrochloride

収率 42.2%

溶媒

water

methylene chloride

反応条件

後処理

1. 1
   温度After the temperature was raised gradually to 0° C. over a period of 1.5 hours
2. 2
   ろ過The precipitates were collected by filtration
3. 3
   洗浄washed with a small amount of isopropyl alcohol

実験手順

To a solution of benzyl 7β-(2-phenoxyacetamido)-2-oxo-3-cephem-4-carboxylate (294 mg) in methylene chloride (7 ml) were added successively N,N-dimethylaniline (0.17 ml) and phosphorus pentachloride (281 mg) at -35° C. The mixture was stirred for 1.5 hours at -35° to -30° C. and cooled to -50° C. and then thereto was added methanol (0.57 ml). After the temperature was raised gradually to 0° C. over a period of 1.5 hours, water (0.5 ml) was added. The precipitates were collected by filtration and washed with a small amount of isopropyl alcohol to give benzyl 7βamino-2-oxo-3-cephem-4-carboxylate hydrochloride (96.5 mg).

出典