反应详情

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.).

1. concentrationAfter the mixture was concentrated in vacuo
2. additionthe residue was diluted with water (200 ml)
3. extractionextracted with ethyl acetate (200 ml)
4. washThe extract was washed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)