反应详情

温度

100 °C

To a solution of 2.60 g (8.06 mmol) [4-methoxy-7-(tetrahydro-pyran-2-yl)-benzothiazol-2-yl]-carbamic acid methyl ester in 100 ml ethylene glycol was added 100 ml 2 N NaOH and the mixture was heated at 100° C. for 3 h. After cooling to room, the reaction mixture was poured into water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate and concentrated in vacuo. Flash chromatography (acetone/hexane 1/4-1/2) afforded 1.70 g (80%) 4-methoxy-7-(tetrahydro-pyran-2-yl)-benzothiazol-2-ylamine as a white solid. ES-MS m/e (%): 265 (M+H+, 100).

1. temperatureAfter cooling to room
2. extractionextracted three times with dichloromethane
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. concentrationconcentrated in vacuo