HRID242863

反应详情

EQUATION

反应方程式

HRID 242863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methanesulfonyl chloride (158 μL, 2.04 mmol) was added dropwise to a solution of (3-o-tolylbenzo[b]thiophen-2-yl)methanol (432 mg, 1.70 mmol) and DIPEA (385 μL, 2.21 mmol) in anhydrous DCM (10 mL) at RT. Stirring at RT was continued for 18 h then the reaction mixture was washed with water, then dried (Na2SO4) and concentrated in vacuo affording (3-o-tolylbenzo[b]thiophen-2-yl)methyl methanesulfonate as a brown oil (424 mg, 75%). 1H NMR (DMSO, 400 MHz): δ 8.05 (1H, d, J=8.04 Hz), 7.45-7.40 (3H, m), 7.38-7.32 (2H, m), 7.21 (1H, d, J=7.40 Hz), 7.12 (1H, d, J=7.98 Hz), 4.82 (1H, d, J=12.41 Hz), 4.76 (1H, d, J=12.41 Hz), 3.32 (3H, s), 1.99 (3H, s)

WORKUP

后处理

  1. washthe reaction mixture was washed with water
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated in vacuo