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
10 mL (130 mmol) trifluoroacetic acid were added to a solution of 1.90 g (5.00 mmol) tert-butyl [3-(4-iodo-imidazol-1-yl)-1,1-dimethyl-propyl]-carbamate in 90 mL dichloromethane at ambient temperature with vigorous stirring. The reaction mixture was stirred for 16 h at ambient temperature and the solvent was eliminated using the rotary evaporator. The residue was taken up in 100 mL sodium hydroxide solution (1M) and 100 mL dichloromethane. The phases were separated and the aqueous phase was extracted three times with 100 mL dichloromethane. The combined organic phases were dried over magnesium sulphate and the solvent was eliminated using the rotary evaporator. 1.37 g (4.91 mmol, 98%) 3-(4-iodo-imidazol-1-yl)-1,1-dimethyl-propylamine were obtained as a colourless oil.
WORKUP
后处理
- customthe rotary evaporator
- customThe phases were separated
- extractionthe aqueous phase was extracted three times with 100 mL dichloromethane
- dry with materialThe combined organic phases were dried over magnesium sulphate
- customthe rotary evaporator