HRID1699231
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 3 hours
- customThe mixture was evaporated down in vacuo
- dissolutionthe residue remaining was dissolved in a little water
- additionby the addition of solid potassium carbonate
- extractionIt was extracted thoroughly with ethyl acetate
- dry with materialthe combined extracts were dried over sodium sulphate
- customevaporated down in vacuo
- customThe residue was thoroughly triturated with diisopropylether
- customyielded 4.2 g (89.7% of theory) of colourless crystals of melting point 114° C.