HRID1655895

反应详情

EQUATION

反应方程式

HRID 1655895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 2-(4-cyanomethyl-3,4-dihydro-3-oxo-2H-1,4-benzothiazin-2-yl)acetate (580 mg) and 474 mg of 2-amino-4,6-difluorothiophenol hydrochloride were added to 4 ml of anhydrous ethanol, the mixture was heated to reflux under argon atmosphere. After 15 hours, the solvent was distilled off. Water was added to the mixture, and extracted with ethyl acetate. After the drying of the organic layer over anhydrous magnesium sulfate, the solvent was distilled off. The resulting oily matter was subjected to alumina column chromatography. Elution with hexane-ehtyl acetate gave 660 mg of the title compound. The structural formula and physical data of this compound are shown in Table 19.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux under argon atmosphere
  3. distillationthe solvent was distilled off
  4. additionWater was added to the mixture
  5. extractionextracted with ethyl acetate
  6. dry with materialAfter the drying of the organic layer over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off
  8. washElution with hexane-ehtyl acetate