HRID1768040

反应详情

EQUATION

反应方程式

HRID 1768040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux temperature for 12 h
  2. customwith continuous removal of water by use of a Dean-Stark trap (a water
  3. customThe reaction mixture was evaporated
  4. custompurified by chromatography on silica gel (eluent:heptane/ethyl acetate 5:1)
  5. additionAll fractions containing the product
  6. customwere evaporated
  7. customthe crystallized material isolated by filtration
  8. customdried