反应详情

970 mg of (-)-cis-2-(4-methoxyphenyl)-3-(4-chloro-3-nitrobenzoyloxy)-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are dissolved in 20 ml of acetone, and 690 mg of potassium carbonate and 410 mg of 2-(N-methyl-N-ethylamino)ethyl chloride hydrochloride are added thereto. The mixture is refluxed for 3 hours under stirring. After the reaction, the mixture is evaporated under reduced pressure to remove solvent. Ethyl acetate is added to the residue, and the mixture is washed with water. The ethyl acetate solution is dried and evaporated under reduced pressure to remove solvent. 180 mg of oxalic acid and 10 ml of acetone are added to the residue, and the mixture is heated to make a clear solution. The clear solution is allowed to stand. Crystalline precipitates are collected by filtration and dried, whereby 1.06 g of (+)-cis-2-(4-methoxyphenyl)-3-(4-chloro-3-nitrobenzoyloxy)-5-[2-(N-methyl-N-ethylamino)ethyl]-2,3-dihydro-1,5-benzothiazepin-4(5H)-one oxalate are obtained as colorless needles. Yield: 80%.

1. temperatureThe mixture is refluxed for 3 hours
2. customAfter the reaction
3. customthe mixture is evaporated under reduced pressure
4. customto remove solvent
5. additionEthyl acetate is added to the residue
6. washthe mixture is washed with water
7. dry with materialThe ethyl acetate solution is dried
8. customevaporated under reduced pressure
9. customto remove solvent
10. addition180 mg of oxalic acid and 10 ml of acetone are added to the residue
11. temperaturethe mixture is heated
12. customCrystalline precipitates
13. filtrationare collected by filtration
14. customdried