反应详情

A solution of methanesulphonyl chloride (3.43 g) in dichloromethane (30 ml) was added dropwise at room temperature to a stirred solution of 6-chloro-2,3,4,5-tetrahydro-1,4-benzothiazepine (5.2 g, prepared in a similar manner to its hydrochloride, Example 1 above) and triethylamine (3.03 g, 0.03 ml) in dichloromethane (100 ml). The reaction mixture was stirred at room temperature for one hour, washed with water, dried and the solvent was removed by evaporation. Purification of the residue by flash chromatography using dichloromethane as eluent gave 6-chloro-4-methylsulphonyl-2,3,4,5-tetrahydro-1,4-benzothiazepine, which was recrystallised from hexane. Yield 6.06 g (m.p. 85°-86° C.).

1. washwashed with water
2. customdried
3. customthe solvent was removed by evaporation
4. customPurification of the residue by flash chromatography