Methylamine → 1-Methylamino-3-phenoxy-propan-2-ol
反応式
[O:1]1[CH:3]([CH2:4][O:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH2:2]1.[CH3:12][NH2:13]>C(O)C.O>[CH3:12][NH:13][CH2:2][CH:3]([OH:1])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1参加物
5
実験手順
To a solution of 1,2-epoxy-3-phenoxypropane (15 g), in ethanol (50 ml) was added 25-30% methylamine in water (50 ml) and the mixture heated under reflux for 1 h. The ethanol was removed in vacuo and the residue acidified with 2 N hydrochloric acid. The aqueous solution was extracted with ethyl acetate then made alkaline with 2 N sodium hydroxide and extracted into ether. The combined ethereal extracts were dried (Na2SO4), filtered and evaporated to give a semi-solid (14.8 g). The product was distilled in vacuo to give the title compound as white crystals b.p. 110°/0.07 mm, m.p. 74°-77° (9 g).
後処理
- temperaturethe mixture heated
- temperatureunder reflux for 1 h
- customThe ethanol was removed in vacuo
- extractionThe aqueous solution was extracted with ethyl acetate
- extractionextracted into ether
- dry with materialThe combined ethereal extracts were dried (Na2SO4)
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-34f2d98842cb476c9295eb6af4412459
- 出典データセット
- uspto-grants-1984_05
- 特許番号
- US04447428
反応ノート
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