反应详情

To a stirred suspension of 17 mg (0.06 mmol) 7-methoxy-4-(tetrahydro-pyran-4-yl)-thiazolo[5,4-c]pyridin-2-ylamine and 0.015 ml (0.19 mmol) pyridine in 1.5 ml dichloromethane and 0.5 ml tetrahydrofuran was added 0.009 ml (0.07 mmol) phenyl chloroformate and stirring continued at 50° C. for 1 h. 37 mg (0.32 mmol) 4-(hydroxymethyl)piperidine was then added and stirring continued at 50° C. for a further 1 h. The reaction mixture was then concentrated in vacuo. Flash chromatography (methanol/dichloromethane 1/40 then 1/20) afforded 11 mg (42%) 4-hydroxymethylpiperidine-1-carboxylic acid [7-methoxy-4-(tetrahydro-pyran-4-yl)-thiazolo[5,4-c]pyridin-2-yl]-amide as a white crystalline solid. ES-MS m/e (%): 407 (M+H+, 100).

1. stirringstirring
2. waitcontinued at 50° C. for a further 1 h
3. concentrationThe reaction mixture was then concentrated in vacuo