HRID1244079
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customquenched with saturated NH4Cl (40 mL)
- extractionThe solution was extracted with EtOAc (2×25 mL)
- washthe extracts were washed with brine
- dry with materialdried with MgSO4
- concentrationconcentrated