反応式
[CH2:1]([O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])[CH3:2].[CH2:11]([N:18]1[CH2:23][CH2:22][O:21][CH:20]([CH2:24][O:25][S:26]([C:29]2[CH:34]=[CH:33][C:32]([CH3:35])=[CH:31][CH:30]=2)(=[O:28])=[O:27])[CH2:19]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CCOCC>[C:32]1([CH3:35])[CH:31]=[CH:30][C:29]([S:26]([OH:28])(=[O:25])=[O:27])=[CH:34][CH:33]=1.[CH2:11]([N:18]1[CH2:23][CH2:22][O:21][CH:20]([CH2:24][NH:6][C:5]2[CH:7]=[CH:8][CH:9]=[CH:10][C:4]=2[O:3][CH2:1][CH3:2])[CH2:19]1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1参加物
反応条件
- 温度
- 95 °C
実験手順
A mixture of 2-ethoxyaniline (14.0 g.) and 4-benzyl-2-toluene-p-sulphonyloxymethylmorpholine (18.6 g.) is stirred and heated on the steam bath (95° C.) under nitrogen for 24 hours. The mixture is cooled and ether added. The solid thus obtained is collected and crystallised from ethyl acetate to give 4-benzyl-2-(2-ethoxyanilino)methylmorpholine toluene-p-sulphonate, m.p. 127° C. The toluene sulphonate salt is converted into the corresponding dihydrochloride by basifying it with dilute sodium hydroxide solution, extracting the base into ether (3× 200 ml.), washing the ethereal extract with water and then drying it over anhydrous magnesium sulphate followed by filtration and treatment of the ethereal solution of base with ethereal hydrochloric acid solution. The 4-benzyl-2-(2-ethoxyanilino)-methylmorpholine dihydrochloride melts at 226° C. after crystallisation from methanol/ethyl acetate.
後処理
- temperatureThe mixture is cooled
- customThe solid thus obtained
- customis collected
- customcrystallised from ethyl acetate
出典と根拠
- ORDレコード
- ord-d7512c75706848f79c8959a5584299b7
- 出典データセット
- uspto-grants-1977_06
- 特許番号
- US04029786
関連ノート
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