反应详情

2.71 g of (-)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-benzyloxycarbonyl-N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are dissolved in 30 ml of ethanol, and the solution is saturated with gaseous hydrogen chloride under ice-cooling. The saturated solution is stirred at room temperature for 20 hours. The solution is evaporated under reduced pressure at a temperature below 35° C. to remove solvent. The residue is dissolved in benzene, and the solution is extracted with conc. HCl-H2O. The aqueous layer is collected, washed with benzene, alkalized with potassium carbonate and then extracted with chloroform. The extract is washed with water, dried and then evaporated to remove solvent. Isopropyl ether is added to the residue, and crystalline precipitates are collected by filtration. 1.83 g of (-)-cis-2-(4-methoxyphenyl)-3-hydroxy-5-[2-(N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are obtained.

1. temperaturecooling
2. customThe solution is evaporated under reduced pressure at a temperature below 35° C.
3. customto remove solvent
4. dissolutionThe residue is dissolved in benzene
5. extractionthe solution is extracted with conc. HCl-H2O
6. customThe aqueous layer is collected
7. washwashed with benzene
8. extractionextracted with chloroform
9. washThe extract is washed with water
10. customdried
11. customevaporated
12. customto remove solvent
13. additionIsopropyl ether is added to the residue
14. customcrystalline precipitates
15. filtrationare collected by filtration