反应详情

3.01 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are dissolved in 50 ml of pyridine, and 2.31 g of 2-chloro-4-nitrobenzoyl chloride are added thereto under ice-cooling and stirring. The mixture is stirred at room temperature overnight. The mixture is poured into ice-water and then extracted with ethyl acetate. The extract is washed with 10% hydrochloric acid and water, dried and then evaporated under reduced pressure to remove solvent. The residue is purified by silica gel chromatography (solvent, chloroform:methanol=100:1). 4.81 g of (-)-cis-2-(4-methoxyphenyl)-3-(2-chloro-4-nitrobenzoyloxy)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained as a pale yellow powder. Yield: 99%.

1. temperatureunder ice-cooling
2. stirringThe mixture is stirred at room temperature overnight
3. extractionextracted with ethyl acetate
4. washThe extract is washed with 10% hydrochloric acid and water
5. customdried
6. customevaporated under reduced pressure
7. customto remove solvent
8. customThe residue is purified by silica gel chromatography (solvent, chloroform:methanol=100:1)