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
N-Methoxy-N-methyl-trans-4-{[tert-butoxycarbonyl-(4-tert-butylcyclohexyl)amino]methyl}benzamide (1.0 g, 2.3 mmol) was dissolved in DCM (10 ml), and TFA (10 ml) was added. The reaction mixture was stirred at ambient temperature for 2 hours and then taken to dryness by rotary evaporation. The crystal-line residue was then dissolved in ethyl acetate (100 ml), and the organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml). The combined water phases were back extracted once with ethyl acetate (100 ml); and the combined organic phases dried with anhydrous sodium sulphate. Solvent was removed by rotary evaporation, to leave the title product as fine white crystals. Yield: 760 mg (99%).
WORKUP
后处理
- customtaken to dryness by rotary evaporation
- dissolutionThe crystal-line residue was then dissolved in ethyl acetate (100 ml)
- washthe organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml)
- extractionThe combined water phases were back extracted once with ethyl acetate (100 ml)
- dry with materialand the combined organic phases dried with anhydrous sodium sulphate
- customSolvent was removed by rotary evaporation