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
- concentrationThe solution was concentrated in vacuo
- customthe residue partitioned between ethyl acetate and dilute sodium hydroxide
- concentrationThe ethyl acetate layer was concentrated
- 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-61e89085760f418e9d9dad7e02680453
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04642343
関連ノート
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