HRID1471019

反应详情

EQUATION

反应方程式

HRID 1471019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with EtOAc (3×150 mL)
  2. washThe combined organics were washed with H2O and Brine
  3. dry with materialThe organic was then dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification by chromatography (silica gel, 20% EtOAc in Hexanes)