HRID1815105
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
2-(5-Isopropoxy-3-trifluoromethyl-pyrazol-1-yl)-5-methanesulfonyl-pyridine (105 mg) and NCS (N-chlorosuccinimide) (200 mg) were dissolved in DMF under nitrogen, and the reaction mixture was stirred at room temperature for 2.5 days. The reaction mixture was then diluted with 2:1 ethyl acetate:benzene solution (100 ml), and washed with 0.5 N sodium hydroxide solution (100 ml), water (100 ml), and brine (100 ml). The organic layer was dried with sodium sulfate, and the solvent was evaporated in vacuo to give the crude product which was purified by recrystallization from 2:1 of isooctane:methylene chloride to afford the title compound (13 mg, 11%, MS: 384.1).
WORKUP
后处理
- washbenzene solution (100 ml), and washed with 0.5 N sodium hydroxide solution (100 ml), water (100 ml), and brine (100 ml)
- dry with materialThe organic layer was dried with sodium sulfate
- customthe solvent was evaporated in vacuo
- customto give the crude product which
- customwas purified by recrystallization from 2:1 of isooctane