Acetyl bromide → 1-Acetyl-3-hydroxypyrid-2-one
反応式
[OH:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9](Br)(=[O:11])[CH3:10]>O>[C:9]([N:3]1[CH:4]=[CH:5][CH:6]=[C:7]([OH:8])[C:2]1=[O:1])(=[O:11])[CH3:10]参加物
4
実験手順
2,3-Dihydroxypyridine (5.55 g) is refluxed with acetylbromide (10 ml) overnight. The reaction mixture is allowed to cool and water (10 ml) is added. The resulting suspension is extracted with methylene chloride and the methylene chloride solution is dried over Na2SO4 and evaporated. The resultant residue is recrystallised from petroleum ether (80°-100° C.) to give 1-acetyl-3-hydroxypyrid-2-one as white crystals (2.8 g), m.p. 140°-141° C.; νmax (nujol) 1680, 3120 cm-1 ; δ(d6DMSO), 2.2 (s, 3H), 6.1 (t, 1H), 6.65 (m, 1H), 7.2 (d, 1H).
後処理
- temperatureto cool
- extractionThe resulting suspension is extracted with methylene chloride
- dry with materialthe methylene chloride solution is dried over Na2SO4
- customevaporated
- customThe resultant residue is recrystallised from petroleum ether (80°-100° C.)
出典と根拠
- ORDレコード
- ord-6e9525b9191d448a8bfaae6cd7b9a16a
- 出典データセット
- uspto-grants-1987_03
- 特許番号
- US04650793
反応ノート
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