反应详情

温度

10 °C

In 700 ml of dimethylformamide is dissolved 54.8 g of trans-3-amino-2-phenyl-2,3-dihydro-1,5-benzothiazepin-4(5H)-one. To this solution is added 8.8 g of 60% sodium hydride under ice-cooling. The reaction temperature is gradually elevated to room temperature, and the mixture is stirred for 1.5 hours. After the reaction mixture is again cooled to about 10° C., 100 ml of a dimethylformamide solution containing 25.5 ml of ethyl bromoacetate is added dropwise. After the reaction temperature is elevated again to room temperature, the mixture is stirred for 5 hours and then concentrated under reduced pressure. By adding ice-water and chloroform to the residue, the organic substance is extracted. After the chloroform layer is washed with water and dried, the solvent is distilled off under reduced pressure. By adding a mixed solution of isopropyl ether and isopropyl alcohol to the residue, the crystallization is effected. The resulting crystals are collected by filtration to give 37 g of ethyl trans-3-amino-4-oxo-2-phenyl-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate.

1. temperaturecooling
2. customis gradually elevated to room temperature
3. additionis added dropwise
4. customis elevated again to room temperature
5. stirringthe mixture is stirred for 5 hours
6. concentrationconcentrated under reduced pressure
7. additionBy adding ice-water and chloroform to the residue
8. extractionthe organic substance is extracted
9. washAfter the chloroform layer is washed with water
10. customdried
11. distillationthe solvent is distilled off under reduced pressure
12. additionBy adding a mixed solution of isopropyl ether and isopropyl alcohol to the residue
13. customthe crystallization
14. filtrationThe resulting crystals are collected by filtration