反应详情

A solution of 0.88 g of 2-chloro-4-nitrobenzoyl chloride in 3 ml of methylene chloride is dropwise added at room temperature to a mixture of 1.41 g of (+)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-methyl-N-ethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one hydrochloride, 15 ml of methylene chloride and 1 ml of triethylamine. The mixture is stirred for one hour. After the reaction, the mixture is evaporated to remove solvent. The residue is extracted with ethyl acetate, and the extract is washed with water, dried and then evaporated to remove solvent. The oil thus obtained is converted to its oxalate and then recrystallized from ethanol. 1.83 g of (+)-cis-2-(4-methoxyphenyl)-3-(2-chloro-4-nitrobenzoyloxy)-5-[2-(N-methyl-N-ethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one oxalate are thereby obtained as colorless needles. Yield: 83.5%.

1. customAfter the reaction
2. customthe mixture is evaporated
3. customto remove solvent
4. extractionThe residue is extracted with ethyl acetate
5. washthe extract is washed with water
6. customdried
7. customevaporated
8. customto remove solvent
9. customThe oil thus obtained
10. customrecrystallized from ethanol