HRID1768040
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
4.10 g (15.0 mmol) 3-(4-pentafluorosulfanyl-phenyl)-acrylamide, 2.37 g (18.7 mmol) dichloro acetone and 25.0 ml toluene were kept at reflux temperature for 12 h with continuous removal of water by use of a Dean-Stark trap (a water separator used in chemical reactions). The reaction mixture was evaporated and purified by chromatography on silica gel (eluent:heptane/ethyl acetate 5:1). All fractions containing the product were evaporated and the residue stirred with 10 ml isohexane, the crystallized material isolated by filtration dried. 4.40 g (85%) 4-Chloromethyl-2-[2-(4-pentafluoromsulfanyl-phenyl)-vinyl]-oxazole.
WORKUP
后处理
- temperatureat reflux temperature for 12 h
- customwith continuous removal of water by use of a Dean-Stark trap (a water
- customThe reaction mixture was evaporated
- custompurified by chromatography on silica gel (eluent:heptane/ethyl acetate 5:1)
- additionAll fractions containing the product
- customwere evaporated
- customthe crystallized material isolated by filtration
- customdried