HRID1699231

反应详情

EQUATION

反应方程式

HRID 1699231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6.0 g (0.0158 mol) of N-[3-[[[1-(phenylmethyl)-4-piperidinyl]amino]methyl]-2-pyridinyl]-2,2-dimethylpropanamide and 100 ml of conc. hydrochloric acid was refluxed for 3 hours. The mixture was evaporated down in vacuo, the residue remaining was dissolved in a little water and made alkaline by the addition of solid potassium carbonate. It was extracted thoroughly with ethyl acetate, the combined extracts were dried over sodium sulphate and evaporated down in vacuo. The residue was thoroughly triturated with diisopropylether and yielded 4.2 g (89.7% of theory) of colourless crystals of melting point 114° C.

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. customThe mixture was evaporated down in vacuo
  3. dissolutionthe residue remaining was dissolved in a little water
  4. additionby the addition of solid potassium carbonate
  5. extractionIt was extracted thoroughly with ethyl acetate
  6. dry with materialthe combined extracts were dried over sodium sulphate
  7. customevaporated down in vacuo
  8. customThe residue was thoroughly triturated with diisopropylether
  9. customyielded 4.2 g (89.7% of theory) of colourless crystals of melting point 114° C.