HRID629926

反应详情

EQUATION

反应方程式

HRID 629926 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 1-4 (0.40 g, 1.58 mmol), Pd(OAc)2 (0.02 g, 0.08 mmol), xphos (0.074 g, 0.16 mmol) in dioxane (12 mL) was added 3-cyanopropylzinc bromide 0.5M solution in THF (12.6 mL, 6.3 mmol) and the resulting mixture was microwave irradiated for 30 minutes at 100° C. The reaction was allowed to cool and partitioned between ethyl acetate and water. The organic phase was concentrated and flash column separation using a 0-60% ethyl acetate/hexane gradient gave 38-1. (0.42 g, 94%). LRMS (ES) (M+H)+: observed=287.2, calculated=287.4.

WORKUP

后处理

  1. customthe resulting mixture was microwave irradiated for 30 minutes at 100° C
  2. temperatureto cool
  3. custompartitioned between ethyl acetate and water
  4. concentrationThe organic phase was concentrated
  5. customflash column separation
  6. customgave 38-1