HRID2104472

反应详情

EQUATION

反应方程式

HRID 2104472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Diethyl ethoxymethylenemalonate (compound III, 50.4 mL, 249.3 mmol) and 2-(Trifluoromethyl)aniline (compound II, 31 mL, 249.3 mmol) was taken into toluene (250 mL) and refluxed overnight twice. Toluene was evaporated and the resulting liquid was taken into hexane and allowed to sit in a freezer for 1 hour. A white solid crashed out and was filtered and dried to yield 69.73 g (84.4%) of the title compound as white crystals. MS ESI (m/z) 332 ([M+H]+); MS ESI (m/z) 330 ([M−H]−); Anal Calcd. For C15H16F3NO4: C, 54.38; H, 4.87; N, 4.23. Found: C, 54.49; H, 4.68; N, 4.06.

WORKUP

后处理

  1. temperaturerefluxed overnight twice
  2. customToluene was evaporated
  3. filtrationwas filtered
  4. customdried