반응 #1906

반응 방정식

ethyl 3-[N-[4-chloro-2-(4-benzyloxy-α-hydroxy-2-methoxybenzyl)-phenyl]-N-neopentylcarbamoyl]acrylate

potassium carbonate

→

ethyl trans-5-(4-benzyloxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

수율 81.7%

용매

ethanol

반응 조건

후처리

1. 1
   농축After the mixture was concentrated in vacuo
2. 2
   workup.ADDITIONthe residue was diluted with water (200 ml)
3. 3
   추출extracted with ethyl acetate (200 ml)
4. 4
   세척The extract was washed with water
5. 5
   건조dried over magnesium sulfate
6. 6
   농축concentrated in vacuo
7. 7
   기타The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)

실험 절차

To a mixture of ethyl 3-[N-[4-chloro-2-(4-benzyloxy-α-hydroxy-2-methoxybenzyl)-phenyl]-N-neopentylcarbamoyl]acrylate (12 g), potassium carbonate (5.9 g) and ethanol (150 ml) was stirred for 24 h. After the mixture was concentrated in vacuo, the residue was diluted with water (200 ml) and extracted with ethyl acetate (200 ml). The extract was washed with water, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to give ethyl trans-5-(4-benzyloxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (9.8 g) as needles (mp=130°-131° C.).

출처