HRID1060525

反应详情

EQUATION

反应方程式

HRID 1060525 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound of Step C (0.7 g, 2 mmol), 3-trifluoromethylpyrazole (0.27 g, 2 mmol) and potassium carbonate (0.83 g, 6 mmol) were suspended in 10 mL of acetonitrile and heated to reflux for 1 h. The salts were filtered and the acetonitrile was removed under reduced pressure. The residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (85:15) to afford 0.52 g of the title compound of Step D, a compound of this invention, as a white solid melting at 112-114° C. 1H NMR (CDCl3): δ2.39 (s, 3H), 5.53 (s, 2H), 6.62 (d, 1H), 7.6-7.8 (m, 3H), 8.44 (d, 2H), 8.6 (s, 1H).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 1 h
  3. filtrationThe salts were filtered
  4. customthe acetonitrile was removed under reduced pressure
  5. customThe residue was purified by chromatography on silica gel eluting with hexanes/ethyl acetate (85:15)