HRID1409311

反应详情

EQUATION

反应方程式

HRID 1409311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-6-fluoro-4-(1H-pyrazol-5-yl)benzonitrile hydrochloride (201 mmol, 51.8 g) was dissolved in THF (510 ml). Sodium hydroxide 50% (401 mmol, 32.1 g) was added and the resulting mixture was stirred at RT for 3 h. Almost all the solvents were evaporated and water was added to the residue. The mixture was stirred overnight at RT. The precipitate was removed by filtration the solid was flushed twice with water. The solid was dried under vacuum. 35.8 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 7.05 (d, 1H), 7.88-7.97 (m, 2H), 8.02-8.07 (m, 1H), 13.37 (bs, 1H).

WORKUP

后处理

  1. customAlmost all the solvents were evaporated
  2. additionwater was added to the residue
  3. stirringThe mixture was stirred overnight at RT
  4. customThe precipitate was removed by filtration the solid
  5. customwas flushed twice with water
  6. customThe solid was dried under vacuum