HRID1012091

反应详情

EQUATION

反应方程式

HRID 1012091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of (3,4-dinitro-phenyl)-morpholin-4-yl-methanone (2.84 g) in dry THF (50 ml) was added NaBH4 (954 mg) followed drop-wise by BF3.Et2O (3.2 ml). The mixture was stirred at ambient temperature for 3 hours and then quenched though addition of MeOH. The mixture was reduced in vacuo, partitioned between EtOAc and water and the organic portion washed with brine, dried (MgSO4) and reduced in vacuo. The residue was purified via flash column chromatography eluting with EtOAc to give 4-(3,4-dinitro-benzyl)-morpholine (1.08 g).

WORKUP

后处理

  1. customquenched though addition of MeOH
  2. custompartitioned between EtOAc and water
  3. washthe organic portion washed with brine
  4. dry with materialdried (MgSO4)
  5. customThe residue was purified via flash column chromatography
  6. washeluting with EtOAc