HRID634767

反应详情

EQUATION

反应方程式

HRID 634767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of trans-[4-(4-benzyloxy-phenyl)-cyclohexyl]-(3-phenyl-propyl)-amine (0.4 g, 1.0 mmol), 36.5% aq. formaldehyde (0.12 ml) and MeOH (7 ml) was stirred overnight at RT. Excess sodium borohydride was then added, and stirring was continued for 2 h. Evaporation of the solvent, addition of H2O, extraction with CH2Cl2, drying of the organic layer with Na2SO4, evaporation of the solvent and purification of the residue by chromatography over SiO2 (Merck 230-400 mesh) eluting with CH2Cl2—MeOH—25% aq. NH3 140:10:1 trans-[4-(4-benzyloxy-phenyl)-cyclohexyl]-methyl-(3-phenyl-propyl)-amine (0.41 g, 99%) as a colorless oil. MS: m/e=413 (M+).

WORKUP

后处理

  1. stirringstirring
  2. waitwas continued for 2 h
  3. customEvaporation of the solvent, addition of H2O, extraction with CH2Cl2
  4. dry with materialdrying of the organic layer with Na2SO4, evaporation of the solvent and purification of the residue by chromatography over SiO2 (Merck 230-400 mesh)
  5. washeluting with CH2Cl2—MeOH—25% aq. NH3 140:10:1 trans-[4-(4-benzyloxy-phenyl)-cyclohexyl]-methyl-(3-phenyl-propyl)-amine (0.41 g, 99%) as a colorless oil