反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 7-[(2-fluoro-pyridine-3-carbonyl)-amino]-4,4-dimethyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (0.187 g), C-(2,3-dihydro-1H-pyrrolo[2,3-b]pyridin-4-yl)-methylamine HCl salt (0.098 g, step B), DIEA (1.0 mL) and IpOH (1.5 mL) was subjected to a Microwave condition (170° C., 1000 s). Solvent was removed and the residue was purified by chromatography through silica gel (70 g, 1-4% MeOH/CH2Cl2 with 1% NH4OH, stepwise gradient) to afford 7-({2-[(2,3-dihydro-1H-pyrrolo[2,3-b]pyridin-4-ylmethyl)-amino]-pyridine-3-carbonyl}-amino)-4,4-dimethyl-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester as cream color solid. MS: (ES+) 529 (M+H). Calc'd. for C30H36N6O3—528.65.
WORKUP
后处理
- customwas subjected to a Microwave condition (170° C., 1000 s)
- customSolvent was removed
- customthe residue was purified by chromatography through silica gel (70 g, 1-4% MeOH/CH2Cl2 with 1% NH4OH, stepwise gradient)