HRID1471019
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
PROCEDURE
实验过程
A mixture of Example 42C (1.0 g, 1.948 mmol) and CuCN (523 mg, 5.84 mmol) in Dimethylformamide (9.5 mL) was heated to 160° C. for 4.5 hours in a microwave. Mixture was poured into a dimethylamine/H2O mixture (1/10) and extracted with EtOAc (3×150 mL). The combined organics were washed with H2O and Brine. The organic was then dried (MgSO4), filtered and concentrated. Purification by chromatography (silica gel, 20% EtOAc in Hexanes) afforded 395 mg (50%) of the title compound. MS (ESI) m/z 406 (M+H)+.
WORKUP
后处理
- extractionextracted with EtOAc (3×150 mL)
- washThe combined organics were washed with H2O and Brine
- dry with materialThe organic was then dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customPurification by chromatography (silica gel, 20% EtOAc in Hexanes)