反应详情

1.42 g of (-)-cis-2-(4-methoxyphenyl)-3-acetoxy-5-[2-(N-benzyloxycarbonyl-N-methylamino)ethyl]-8-chloro-2,3-dihydro-1,5-benzothiazepin-4(5H)-one are dissolved in a mixture of 15 ml of conc. HCl and 15 ml of methanol. The solutin is saturated with gaseous hydrogen chloride, and the saturated solution is stirred at room temperature for 19 hours. The mixture is evaporated under reduced pressure at a temperature below 35° C. to remove solvent. The residue is dissolved in 10% HCl. The solution is washed with ether, alkalized with potassium carbonate and then extracted with chloroform. The extract is washed with water, dried and then evaporated to remove solvent. A mixture of ethanol and ethyl acetate is added to the residue, and crystalline precipitates are collected by filtration. 770 mg 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. customThe mixture is evaporated under reduced pressure at a temperature below 35° C.
2. customto remove solvent
3. dissolutionThe residue is dissolved in 10% HCl
4. washThe solution is washed with ether
5. extractionextracted with chloroform
6. washThe extract is washed with water
7. customdried
8. customevaporated
9. customto remove solvent
10. additionA mixture of ethanol and ethyl acetate
11. additionis added to the residue
12. customcrystalline precipitates
13. filtrationare collected by filtration