HRID2088762

反应详情

EQUATION

反应方程式

HRID 2088762 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-nitro-benzaldehyde (10 g, 0.0390 mol), a known compound (which may be prepared as disclosed in European Patent EP 371564) and 3-amino-N-cyclohexyl-N-methyl-propionamide (7.5 g, 0.0410 mol) in 1,2-dichloroethane (250 mL) was stirred at room temperature under nitrogen. Sodium triacetoxyborohydride (8.7 g, 0.0410 mol) was added, and the reaction mixture was stirred for 6 h at room temperature. Saturated NaHCO3 solution (200 mL) was then added. The organic layer was separated, dried, and evaporated. The resulting residue was purified by column chromatography on silica gel (eluent: 99:1 CH2Cl2:MeOH). The purest fractions were combined, and the solvent was evaporated to yield a residue.

WORKUP

后处理

  1. stirringthe reaction mixture was stirred for 6 h at room temperature
  2. customThe organic layer was separated
  3. customdried
  4. customevaporated
  5. customThe resulting residue was purified by column chromatography on silica gel (eluent: 99:1 CH2Cl2:MeOH)
  6. customthe solvent was evaporated
  7. customto yield a residue