HRID1244079

反应详情

EQUATION

反应方程式

HRID 1244079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To (1,1-Dimethyl-4-nitro-but-3-enyl)-carbamic acid tert-butyl ester (2.0 g, 8.2 mmol) in 20 mL of EtOH was added NaBH4 (500 mg, 13.5 mmol). The mixture was stirred 1 h and then quenched with saturated NH4Cl (40 mL). The solution was extracted with EtOAc (2×25 mL), the extracts were washed with brine, dried with MgSO4 and concentrated. Silica gel chromatography (10:1 hexane/EtOAc) gave 1.57 g (78%) of a colorless oil: mass spectru m/e=147 (M−100).

WORKUP

后处理

  1. customquenched with saturated NH4Cl (40 mL)
  2. extractionThe solution was extracted with EtOAc (2×25 mL)
  3. washthe extracts were washed with brine
  4. dry with materialdried with MgSO4
  5. concentrationconcentrated