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
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of phenyl 5-bromothiophene-3-carboxylate, Example 113 (100 mg, 0.35 mmol), (prop-2-ynyloxy)benzene (93 mg, 0.71 mmol), triphenylphosphine (19 mg, 0.071 mmol), dichlorobis(triphenylphosphine)palladium(II) (12 mg, 0.018 mmol), copper iodide (1 mg, 0.006 mmol) and triethylamine (0.74 mL, 5.30 mmol) in N,N-dimethylformamide (1 mL) was stirred under nitrogen in a heavy walled process vial in a microwave synthesizer at about 120° C. for about 25 minutes. The reaction mixture was concentrated under vacuum and the residue was purified by flash column chromatography on silica gel using hexane/ethyl acetate (2:1) as the mobile phase to provide the desired product. MS (DCI-NH3): m/z 352 (M+NH4)+.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under vacuum
- customthe residue was purified by flash column chromatography on silica gel