반응 #4922

반응 방정식

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

용매

ethanol

반응 조건

후처리

1. 1
   농축The solution was concentrated in vacuo
2. 2
   기타the residue partitioned between ethyl acetate and dilute sodium hydroxide
3. 3
   농축The 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

실험 절차

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.

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