HRID242880

反应详情

EQUATION

反应方程式

HRID 242880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-phenylbenzo[b]thiophene-2-carbaldehyde (430 mg, 1.87 mmol) in THF (10 mL) at −78° C. and under a nitrogen atmosphere was added 3.0M methylmagnesium bromide in diethyl ether (1.24 mL) and stirring continued for 30 min. The reaction mixture was quenched with a saturated solution of NH4Cl (20 mL) and slowly warmed to RT. The mixture was extracted with EtOAc (×2) and the combined organic fractions washed with water, dried (Na2SO4) and concentrated in vacuo affording the title compound as a white solid (472 mg, quantitative). 1H NMR (CDCl3, 400 MHz): δ 7.88-7.84 (1H, m), 7.52-7.28 (8H, m), 5.21 (1H, q, J=6.35 Hz), 2.03 (1H, s), 1.59 (3H, d, J=6.63 Hz)

WORKUP

后处理

  1. customThe reaction mixture was quenched with a saturated solution of NH4Cl (20 mL)
  2. extractionThe mixture was extracted with EtOAc (×2)
  3. washthe combined organic fractions washed with water
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo