HRID359264

反应详情

EQUATION

反应方程式

HRID 359264 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a reaction vessel containing a stirred mixture of 3.15 g (13 mmol) of ethyl 2-chloro-4-trifluoromethyl-5-oxazolecarboxylate in 25 ml of toluene, there was added 3 ml (29 mmol) of diethylamine. The reactionmixture was stirred at ambient temperature for 4 hours and then suction filtered. The filtrate was washed with 5% hydrochloric acid, then with saturated brine, then dried over sodium sulfate and concentrated under reduced pressure to yield 3.3 g of a pale yellow oil. This oil was subjected to Kugelrohr distillation (60° C. @ 3 mm Hg) to remove trace amounts of starting material. Further Kugelrohr distillation provided 2.9 g of colorless oil (b.p. 110° C. @ 3 mm Hg) identified in Table I.

WORKUP

后处理

  1. additionTo a reaction vessel containing
  2. filtrationsuction filtered
  3. washThe filtrate was washed with 5% hydrochloric acid
  4. dry with materialwith saturated brine, then dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure