反应详情

温度

0 °C

To a solution of (S)-1-[4-((S)-4-hydroxy-6-aza-spiro[2.5]oct-6-yl)-butyl]-3-methyl-piperazin-2-one (intermediate 27; 50 mg, 0.17 mmol) in tetrahydrofuran (0.5 mL) was added at 0° C. O-2-naphthyl chlorothioformate (38 mg, 0.17 mmol) and triethylamine (17 mg, 0.17 mmol). The ice bath was removed, then after 20 min the reaction mixture was cooled to 0° C. and treated with diethylamine (6 mg, 90 μmol), then concentrated under vacuum. Chromatography (SiO2; dichloromethane/methanol/25% aq. ammonia solution 90:10:0.25) furnished the title compound (52 mg, 64%). Orange oil, MS (ISP)=482.4 (M+H)+.

1. customThe ice bath was removed
2. concentrationconcentrated under vacuum