HRID480379

反应详情

EQUATION

反应方程式

HRID 480379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customtaken to dryness by rotary evaporation
  2. dissolutionThe crystal-line residue was then dissolved in ethyl acetate (100 ml)
  3. washthe organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml)
  4. extractionThe combined water phases were back extracted once with ethyl acetate (100 ml)
  5. dry with materialand the combined organic phases dried with anhydrous sodium sulphate
  6. customSolvent was removed by rotary evaporation