反应详情

To a mixture of (S)-(+)-3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]-2-methyl-1-propanol (8.8 g, 30 mmol), triethylamine (3.2 g, 32 mmol) in dichloromethane (DCM, 150 ml), methanesulfonyl chloride (4 g, 35 mmol) was added dropwise at 0° C. over 10 minutes. The mixture was stirred at room temperature for 1 hour, then concentrated. Triethylamine HCl salt was filtered off with a little DCM as solvent. The crude oil was purified with a flash chromatography column (SiO2, 90 g; eluted with DCM). The colorless oil thus purified weighed 5.28 g (47%) was used immediately in the following step.

1. additionwas added dropwise at 0° C. over 10 minutes
2. concentrationconcentrated
3. filtrationTriethylamine HCl salt was filtered off with a little DCM as solvent
4. customThe crude oil was purified with a flash chromatography column (SiO2, 90 g; eluted with DCM)
5. customThe colorless oil thus purified