HRID1484556

反应详情

EQUATION

反应方程式

HRID 1484556 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 5.4 g (24.0 mmol) (2E)-2-[(3-methyl-1H-indazol-5-yl)methylidene]-3-oxobutanenitrile (Example 2A) and 13.05 g (95.9 mmol) 3-amino-4,4,4-trifluorobut-2-enenitrile [preparation: A. W. Lutz, U.S. Pat. No. 3,635,977; C. G. Krespan, J. Org. Chem. 34, 42 (1969)] in 2-propanol (27 ml) and triethylamine (0.33 ml) was stirred at reflux temperature for 15 h. After cooling, the precipitate was collected by filtration, washed twice with cold 2-propanol and dried under high vacuum to yield 5.98 g (72% of th.) of the racemic title compound as a tan solid.

WORKUP

后处理

  1. custompreparation
  2. temperatureat reflux temperature for 15 h
  3. temperatureAfter cooling
  4. filtrationthe precipitate was collected by filtration
  5. washwashed twice with cold 2-propanol
  6. customdried under high vacuum