HRID390245

反应详情

EQUATION

反应方程式

HRID 390245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-benzoyl-2-nitrobenzaldehyde (0.0058 mol) in THF (100 ml) was hydrogenated with 10% Pd/C (1 g) as a catalyst in the presence of 4% thiophene solution (1 mL). After uptake of H2 (3 equiv), the mixture was put in an autoclave. N-cyclohexyl, N-methyl-propane-1,3-diamine (0.01 mol) and CaH2 (0.5 g) were added and the mixture was reacted under 10 atm of CO2 and 50 atm of H2 at 50° C. for 16 hours. When the reaction was complete, the mixture was purified over silica gel on a glass filter (eluent: 90:10 CH2Cl2:(CH3OH:NH3)). The product fractions were collected and the solvent was evaporated to yield the title compound as a residue.

WORKUP

后处理

  1. customthe mixture was purified over silica gel on a glass
  2. filtrationfilter (eluent: 90:10 CH2Cl2:(CH3OH:NH3))
  3. customThe product fractions were collected
  4. customthe solvent was evaporated