HRID1990731

反应详情

EQUATION

反应方程式

HRID 1990731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 3-chloro-5-trifluoromethoxybenzyl alcohol (6.1 g) 26.9 mmol; see Example 6(v) above) in CH2Cl2 (250 mL) at 0° C. under a nitrogen atmosphere was added DIPEA (4.2 g, 32.3 mmol) and methanesulfonyl chloride (3.4 g, 29.6 mmol). The solution was stirred at 0° C. for 1.5 hours and quenched with H2O. The organics were separated and then washed with H2O (1×), 1N HCl (1×), H2O (1×) and aqueous NaHCO3 (1×) and then dried (Na2SO4), filtered and concentrated to afford the sub-title compound (8.2 g, 99%) as an oil.

WORKUP

后处理

  1. customat 0° C.
  2. customquenched with H2O
  3. customThe organics were separated
  4. washwashed with H2O (1×), 1N HCl (1×), H2O (1×) and aqueous NaHCO3 (1×)
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated