反应详情

温度

0 °C

To a solution of 1,1-dimethylethyl 4-(5-{4-[3-(4-aminophenyl)-1-methyl-1H-pyrazol-4-yl]-1H-pyrrolo[2,3-b]pyridin-2-yl}-2-pyrimidinyl)-1-piperazinecarboxylate (0.326 mmol) in pyridine (8 ml) under argon at 0° C. was added isopropenyl chloroformate (1.31 mmol) portionwise over 3 hours maintaining the reaction temperature at 0° C. The resulting solution was concentrated, purified by reverse-phase. This intermediate was dissolved in THF (10 ml) and dimethylamine (2M in THF, 20 ml) was added. After heating for 2 hours at 50° C., concentration in vacuo provided the title product (27%) as a yellow solid which was used without further purification. ESMS [M+H]+: 623.2.

1. concentrationThe resulting solution was concentrated
2. custompurified by reverse-phase
3. dissolutionThis intermediate was dissolved in THF (10 ml)
4. additiondimethylamine (2M in THF, 20 ml) was added
5. temperatureAfter heating for 2 hours at 50° C.
6. concentrationconcentration in vacuo