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