反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customFrom the mixture obtained solvent
- customis evaporated
- customthe evaporation residue obtained
- customthe mixture obtained
- extractionis extracted with 50 ml of 1 M HCl and brine
- customTwo phases are obtained
- customare separated
- customthe organic layer obtained
- concentrationis concentrated