反应详情

2,3,4,5-Tetrahydro-1,4-benzothiazepine (11 g) and triethylamine (13.5 g) were dissolved in THF (300 ml) and acryloyl chloride (9.5 g) was added dropwise thereto under ice cooling and agitated at room temperature for 30 minutes. A 10% potassium hydroxide aqueous solution was added thereto, agitated at room temperature and thereafter extracted with chloroform. The chloroform phase was washed with a saturated saline solution and dried on sodium sulfate and the solvent was distilled out under reduced pressure. Residue was purified by silica gel column chromatography (Wako Gel C-200, 200 g) and eluted with a mixed solvent of n-hexane (60 parts) +ethyl acetate (40 parts) to give 4-acryloyl-2,3,4,5-tetrahydro-1,4-benzothiazepine (12.59).

1. stirringagitated at room temperature
2. extractionextracted with chloroform
3. washThe chloroform phase was washed with a saturated saline solution
4. customdried on sodium sulfate
5. distillationthe solvent was distilled out under reduced pressure
6. customResidue was purified by silica gel column chromatography (Wako Gel C-200, 200 g)
7. washeluted with a mixed solvent of n-hexane (60 parts) +ethyl acetate (40 parts)