HRID749238

反应详情

EQUATION

反应方程式

HRID 749238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-methoxy-1,3-benzothiazol-2(3H)-one (DE 3017977 A1) (1.92 g) in dry dichloromethane (50 ml) was cooled to ˜5° C. under nitrogen. Acetyl chloride (1.43 ml) and aluminium chloride (3.43 g) were added in one portion, and stirred for 2 h at RT. The reaction was quenched carefully with water, followed by addition of 2N HCl and dichloromethane. The aqueous layer was extracted with dichloromethane, and the combined organic layers were washed with brine and dried (Na2SO4) and evaporated in vacuo to give the title compound (1.92 g). LCMS RT=2.50 min

WORKUP

后处理

  1. customThe reaction was quenched carefully with water
  2. additionfollowed by addition of 2N HCl and dichloromethane
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. washthe combined organic layers were washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated in vacuo