HRID1591935

反应详情

EQUATION

反应方程式

HRID 1591935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.3 g of 2-(3,5-bis-trifluoromethyl-benzenesulfonylamino)-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-5-ium hydrochloride, 1.545 g of 2-fluoro-4-trifluoromethyl-benzamide and 3.3 g of K2CO3 are heated in DMSO at 150° for 5 hours. From the mixture obtained solvent is evaporated, the evaporation residue obtained is dissolved in EtAc/MeOH (9/1) and the mixture obtained is extracted with 50 ml of 1 M HCl and brine. Two phases are obtained and are separated and the organic layer obtained is concentrated and subjected to chromatography. 2-[2-(3,5-Bis-trifluoromethyl-benzenesulfonylamino)-6,7-dihydro-4H-thiazolo-[5,4-c]pyridin-5-yl]-4-trifluoromethyl-benzamide is obtained and is re-crystallized from EtAc.

WORKUP

后处理

  1. customFrom the mixture obtained solvent
  2. customis evaporated
  3. customthe evaporation residue obtained
  4. customthe mixture obtained
  5. extractionis extracted with 50 ml of 1 M HCl and brine
  6. customTwo phases are obtained
  7. customare separated
  8. customthe organic layer obtained
  9. concentrationis concentrated