HRID1631337
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
Tert-butyl phenyl carbonate (0.421 mL, 2.270 mmol) was added to a solution of 2-methylpropane-1,2-diamine (200 mg, 2.270 mmol) in EtOH (4.5 mL) and the reaction mixture was heated at reflux overnight. The mixture was concentrated and the residue diluted in water. The mixture was acidified with 2N HCl to pH 4 and washed with DCM. The aqueous layer was treated with 1M NaOH (2 mL) and extracted with DCM. The combined organic layers were dried with MgSO4, filtered and concentrated to afford tert-butyl 2-amino-2-methylpropylcarbamate (158 mg, 37% yield) as a colorless oil. MS (apci) m/z=188.9 (M+H).
WORKUP
后处理
- temperaturethe reaction mixture was heated
- temperatureat reflux overnight
- concentrationThe mixture was concentrated
- additionthe residue diluted in water
- washwashed with DCM
- additionThe aqueous layer was treated with 1M NaOH (2 mL)
- extractionextracted with DCM
- dry with materialThe combined organic layers were dried with MgSO4
- filtrationfiltered
- concentrationconcentrated