HRID564054

反应详情

EQUATION

反应方程式

HRID 564054 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To 13.0 g (41.6 mmol) 6-bromo-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester in 42 mL 1,4-dioxane is added 817 mg (4.21 mmol) copper(I)-iodide under argon. After flushing with argon, 0.89 mL (8.33 mmol) N,N-dimethylethylen-diamine and 12.5 g (83.3 mmol) sodium iodide is added at RT. The reaction mixture is stirred 14 h at 110° C., is cooled to RT and is diluted with 5% aqueous ammonia-solution. The layers are separated and the aqueous phase is extracted with EtOAc. The combined organic phase is washed with water and is dried over MgSO4, filtered and the solvent is evaporated to give the product.

WORKUP

后处理

  1. additionis added at RT
  2. temperatureis cooled to RT
  3. customThe layers are separated
  4. extractionthe aqueous phase is extracted with EtOAc
  5. washThe combined organic phase is washed with water
  6. dry with materialis dried over MgSO4
  7. filtrationfiltered
  8. customthe solvent is evaporated
  9. customto give the product