HRID2421948

反应详情

EQUATION

反应方程式

HRID 2421948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oxalyl chloride (0.185 g, 1.46 mmol) was added dropwise to a solution of 4-hydroxy-2-(2-methoxyethyl)-5-phenylisothiazol-3(2H)-one 1,1-dioxide (0.250 g, 0.88 mmol) in DCM (15 mL). The mixture was refluxed for 2 days and then evaporated. The residue was dissolved in water and extracted 3 times with dichloromethane. The combined organic layers were washed 2 times with water, dried through a phase separator and evaporated to give the title compound (0.245 g, 92%) as a solid; 1H NMR (500 MHz, CD3OD): δ 7.94-7.97 (m, 2H), 7.58-7.67 (m, 3H), 3.94 (t, 2H), 3.70 (t, 2H), 3.38 (s, 3H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 2 days
  2. customevaporated
  3. dissolutionThe residue was dissolved in water
  4. extractionextracted 3 times with dichloromethane
  5. washThe combined organic layers were washed 2 times with water
  6. customdried through a phase separator
  7. customevaporated