反応 #1883

反応方程式

trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetaldehyde

(ethoxycarbonylmethylene)-triphenylphosphorane

→

trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-crotonic acid

収率 77.1%

溶媒

toluene

反応条件

後処理

1. 1
   workup.DISTILLATIONThe solvent was distilled off
2. 2
   その他the residue was purified by means of a silica gel column chromatography (hexane:ethyl acetate=10:1)

実験手順

In toluene (20 ml) was dissolved trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetaldehyde (1.5 g). To the solution was added (ethoxycarbonylmethylene)-triphenylphosphorane (2.0 g), and the mixture was stirred for 3 hours at 90° C. The solvent was distilled off, and the residue was purified by means of a silica gel column chromatography (hexane:ethyl acetate=10:1) to give ethyl ester of trans-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-crotonic acid (1.28 g) as prisms, m.p.126°-127° C.

出典