反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Zinc cyanide (28 mg, 0.23 mmol) was added to 2-(5-Bromo-pyridin-2-yl)-N-[5-(7-(propan-2-yl)-7H-pyrrolo[2,3-d]pyrimidine-5-carbonyl)-pyridin-3-yl]-acetamide (Example 317, 75 mg, 0.16 mmol) in DMF (2 mL) and the mixture was degassed with argon for 10 minutes. Then tris(dibenzylideneacetone)dipalladium (3 mg, 0.003 mmol) and 1,1′-bis(diphenylphosphino)ferrocene (7 mg, 0.012 mmol) were added and the mixture was heated at 100° C. for 40 mins under microwave irradiation. The mixture was diluted with EtOAc (5 mL) and washed with water (2 mL), brine (2 mL) and dried over sodium sulphate. The filtrate was evaporated in vacuo and purified by preparative TLC (3% MeOH in DCM) to afford the title compound as a light brown solid in 18% yield, 12 mg.
WORKUP
后处理
- customthe mixture was degassed with argon for 10 minutes
- washwashed with water (2 mL), brine (2 mL)
- dry with materialdried over sodium sulphate
- customThe filtrate was evaporated in vacuo
- custompurified by preparative TLC (3% MeOH in DCM)