HRID629926
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
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
- customthe resulting mixture was microwave irradiated for 30 minutes at 100° C
- temperatureto cool
- custompartitioned between ethyl acetate and water
- concentrationThe organic phase was concentrated
- customflash column separation
- customgave 38-1