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

HRID 236169

반응식

HRID 236169 반응식
[CH3:1][NH:2][CH3:3].[Cl:4][CH2:5][CH2:6][CH:7]1[CH2:13][N:12]([CH3:14])[C:11](=[O:15])[C:10]2[CH:16]=[CH:17][CH:18]=[CH:19][C:9]=2[O:8]1>C(O)C>[ClH:4].[CH3:1][N:2]([CH3:3])[CH2:5][CH2:6][CH:7]1[CH2:13][N:12]([CH3:14])[C:11](=[O:15])[C:10]2[CH:16]=[CH:17][CH:18]=[CH:19][C:9]=2[O:8]1

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 137262932-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one

생성물 1

HCID 137263172-[2-(Dimethylamino)ethyl]-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
100 °C

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 ketoneisopropanol mixture. The solution was acidified with hydrogen chloride gas to give the title compound, m.p. 188°-197° C.

후처리

  1. concentrationThe solution was concentrated in vacuo
  2. customthe residue partitioned between ethyl acetate and dilute sodium hydroxide
  3. concentrationThe ethyl acetate layer was concentrated
  4. dissolutionthe residue comprised substantially of the free base of the title compound was dissolved in methyl isobutyl ketoneisopropanol mixture

출처 및 근거

ORD 기록
ord-61e89085760f418e9d9dad7e02680453
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04642343

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