HRID654733

反应详情

EQUATION

反应方程式

HRID 654733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 2,4,4,4-tetrafluoro-3-oxobutanoate (81 g.) in toluene (60 ml) was stirred and heated to 70° C. whereupon ammonia gas was bubbled in until an uptake of 6.8 g. was recorded. The reaction was then set for reflux and water removed azeotropically. Approximately 10 ml of water was removed. After cooling, the solvent was removed under reduced pressure and the residue distilled to give ethyl 3-amino-2,4,4,4-tetrafluoro-2-butenoate b.p. 79°-86° C./20 mm, 44 g.

WORKUP

后处理

  1. customwas bubbled in until an uptake of 6.8 g
  2. temperaturefor reflux
  3. customwater removed azeotropically
  4. customApproximately 10 ml of water was removed
  5. temperatureAfter cooling
  6. customthe solvent was removed under reduced pressure
  7. distillationthe residue distilled