HRID572702

反应详情

EQUATION

反应方程式

HRID 572702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 4-benzyloxy-3-nitro-α-[N-benzyl-N-(1-methyl-2-p-methoxyphenylethyl)aminomethyl]benzyl alcohol (100 gms, 0.19 M) in DMF (500 ml) was added 10% Pd/C. The resulting mass was heated to 40° C. and ammonium formate (36 gms, 0.57 M) was added in lots in 1 hour. The reaction mass was heated slowly to 70-75° C. for 1 hour, then cooled to 50° C. The catalyst was removed by filtration and the clear filtrate evaporated. The residue was stirred in water (500 ml) and basified with liq. Ammonia. The reaction mass was extracted in 1.0-lit toluene, washed organic extract with water, dried on sodium sulfate and evaporated to obtain title compound. (80 gms, 84.21%)

WORKUP

后处理

  1. temperatureThe reaction mass was heated slowly to 70-75° C. for 1 hour
  2. temperaturecooled to 50° C
  3. customThe catalyst was removed by filtration
  4. customthe clear filtrate evaporated
  5. extractionThe reaction mass was extracted in 1.0-lit toluene
  6. washwashed organic
  7. extractionextract with water
  8. customdried on sodium sulfate
  9. customevaporated