HRID1699230

反应详情

EQUATION

反应方程式

HRID 1699230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8.2 g (0.0398 mol) of N-(3-formyl-2-pyridinyl)-2,2-dimethylpropanamide and 7.6 g (0.04 mol) of 4-amino-1-(phenylmethyl)piperidine in 80 ml of methanol was combined in batches with a total of 1.7 g (0.045 mol) of sodium borohydride and refluxed for a total of 24 hours. The solvent was removed in vacuo, the residue was distributed between water and ethyl acetate. The organic phase was dried over sodium sulphate and freed from solvent. The residue was triturated with diisopropylether and suction filtered. 6.0 g (39.6% of theory) of colourless crystals of melting point 138° C. were obtained.

WORKUP

后处理

  1. temperaturerefluxed for a total of 24 hours
  2. customThe solvent was removed in vacuo
  3. dry with materialThe organic phase was dried over sodium sulphate
  4. customThe residue was triturated with diisopropylether and suction
  5. filtrationfiltered
  6. custom6.0 g (39.6% of theory) of colourless crystals of melting point 138° C. were obtained