HRID846057

反应详情

EQUATION

反应方程式

HRID 846057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.3 g (0.045 mol) of 2-phenoxyethanol are added slowly while stirring to a solution of 11 g (0.44 mol) of 2-chloro-5-chlorcarbonyl-4-trifluoromethyl-thiazole in 100 ml of absolute toluene. The solution is then cooled to 0°-5° and 3.6 g (0.045 mol) of triethylamine are added dropwise while stirring. Triethylamine-hydrochloride precipitates from the reaction mixture. After everything is added, the suspension is stirred for 20 hours at room temperature and then poured onto ice-water. The organic phase is separated, dried over sodium sulfate and concentrated in a rotatory evaporator. The residue cristallizes. In order to purify it, the crystals are suspended in petrol-ether, filtered and dried. In this manner 8.7 g (57% of the theoreticl yield) of the title compound are obtained, m.p. 70°-72°.

WORKUP

后处理

  1. temperatureThe solution is then cooled to 0°-5°
  2. customTriethylamine-hydrochloride precipitates from the reaction mixture
  3. additionAfter everything is added
  4. stirringthe suspension is stirred for 20 hours at room temperature
  5. additionpoured onto ice-water
  6. customThe organic phase is separated
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in a rotatory evaporator
  9. customIn order to purify it
  10. filtrationfiltered
  11. customdried