HRID2207058

反应详情

EQUATION

反应方程式

HRID 2207058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
47.5 °C

PROCEDURE

实验过程

Methanol (1.35 Lt) and 3-fluoro-4-morpholinyl nitrobenzene (134 gr) are added into autoclave and followed by Raney Nickel (20.5 gr). The system was flushed with nitrogen and hydrogen gas. The pressure of hydrogen was set to 4.0 kg/cm−2. The reaction mixture was stirred at 45-50° C. under H2 pressure for 8 hrs & the reaction followed by TLC until completion. The reaction mixture was filtered through celite and the filtrate is distilled off evaporate solvent completely U/vacuum at <50° C. temperature. Reaction mass is cooled to 25-30° C. To this DM water (400 ml) is added, Stirred for 1 hr at 25-30° C. The solid is filtered to give 105 gr of 3-fluoro-4-morpholinyl aniline.

WORKUP

后处理

  1. customThe system was flushed with nitrogen and hydrogen gas
  2. filtrationThe reaction mixture was filtered through celite
  3. distillationthe filtrate is distilled off
  4. customevaporate solvent completely U/vacuum at <50° C. temperature
  5. customReaction mass
  6. temperatureis cooled to 25-30° C
  7. stirringStirred for 1 hr at 25-30° C
  8. filtrationThe solid is filtered