HRID349699

反应详情

EQUATION

反应方程式

HRID 349699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 500 mL roundbottom flask equipped with stir bar and 3-way stopcock charged with MeOH/tetrahydrofuran/water (200 mL of 2:1:1) was purged thoroughly with nitrogen. To this was added 1.0 g of 10% Pd/C followed by addition of 10 g (48.0 mmol) of 3-morpholinyl nitrobenzene. The mixture then was stirred under a hydrogen atmosphere for 4 days (1 atm). The reaction was filtered over GF/F filter paper and the filtrate concentrated in vacuo to remove MeOH and THF. The resulting solid was recovered by filtration, washed with water, air dried, then dried in vacuo to give 7.3 g (83% yield) of the desired aniline as beige crystals.

WORKUP

后处理

  1. customA 500 mL roundbottom flask equipped
  2. customwas purged thoroughly with nitrogen
  3. additionTo this was added 1.0 g of 10% Pd/C
  4. stirringThe mixture then was stirred under a hydrogen atmosphere for 4 days (1 atm)
  5. filtrationThe reaction was filtered over GF/F
  6. filtrationfilter paper
  7. concentrationthe filtrate concentrated in vacuo
  8. customto remove MeOH and THF
  9. filtrationThe resulting solid was recovered by filtration
  10. washwashed with water, air
  11. customdried
  12. customdried in vacuo