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

HRID 1194218ノート

反応式

HRID 1194218 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b12fa529d4744e58fe7db407f03aaf8
出典データセット
uspto-grants-1989_03
特許番号
US04812565

反応ノート

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