反应 #4922

反应方程式

dimethylamine

2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one

→

title compound

2-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one hydrochloride

溶剂

ethanol

反应条件

后处理

1. 1
   浓缩The solution was concentrated in vacuo
2. 2
   其他the residue partitioned between ethyl acetate and dilute sodium hydroxide
3. 3
   浓缩The ethyl acetate layer was concentrated
4. 4
   workup.DISSOLUTIONthe residue comprised substantially of the free base of the title compound was dissolved in methyl isobutyl ketone-isopropanol mixture

实验过程

A solution of 9 g (0.2 mole) of dimethylamine in 250 ml of ethanol was added to 24 g (0.1 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one in a steel bomb. The mixture was heated at 100° C. for 18 hrs. The solution was concentrated in vacuo and the residue partitioned between ethyl acetate and dilute sodium hydroxide. The ethyl acetate layer was concentrated and the residue comprised substantially of the free base of the title compound was dissolved in methyl isobutyl ketone-isopropanol mixture. The solution was acidified with hydrogen chloride gas to give the title compound, m.p. 188°-197° C.

来源