反应详情

温度

0 °C

In a round-bottomed flask, (R)-3-{[2-(6-chloro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carbonyl]-amino}-piperidine-1-carboxylic acid tert-butyl ester (138 mg, 0.22 mmol) was suspended in methanol (2 ml). The reaction was cooled to 0° C. and acetyl chloride (0.30 ml, 4.22 mmol) was added dropwise over 10 min. The resultant bright yellow suspension was stirred at room temperature for 50 min. THF (1 ml) and methanol (1 ml) were added and stirred was continued for 1 h at room temperature then the solvent was evaporated at room temperature. The residue was suspended in dichloromethane and washed with saturated Na2CO3-solution. The aqueous layer was extracted with dichloromethane. The organic layers were combined, dried over sodium sulfate, filtered and concentrated to afford 105 mg (90%) of 2-(6-chloro-1-methyl-1H-indazol-3-yl)-5-(2-trimethylsilanyl-ethoxymethyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxylic acid (R)-piperidin-3-ylamide as a light yellow solid.

1. stirringstirred
2. waitwas continued for 1 h at room temperature
3. customthe solvent was evaporated at room temperature
4. washwashed with saturated Na2CO3-solution
5. extractionThe aqueous layer was extracted with dichloromethane
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated