Hydrochloric Acid → 1-(5-Bromo-1,3-thiazol-2-yl)ethan-1-one
反応式
[Br:1][C:2]1[S:6][C:5]([C:7](OC)([O:9]C)[CH3:8])=[N:4][CH:3]=1.Cl>CC(C)=O.O>[Br:1][C:2]1[S:6][C:5]([C:7](=[O:9])[CH3:8])=[N:4][CH:3]=1参加物
5
実験手順
A solution of 5-bromo-2-(1,1-dimethoxyethyl)-1,3-thiazole (35 g) was dissolved in acetone (200 ml) and water (200 ml), was added con. HCl (40 ml). The mixture was stirred for 5 h at room temperature. After concentration to remove acetone, the residue was adjusted to pH=7 by the addition of NaHCO3 and extracted with ether (30 ml×3). The organic layers were washed with brine, dried over Na2SO4 and concentrated to afford 25 g of 1-(5-bromo-1,3-thiazol-2-yl)ethanone as solid (87.4%). 1H-NMR (CDCl3 400 MHz) δ 7.87 (s, 1H, Ar—H), 2.66 (s, 3H, —CH3)
後処理
- concentrationAfter concentration
- customto remove acetone
- additionthe residue was adjusted to pH=7 by the addition of NaHCO3
- extractionextracted with ether (30 ml×3)
- washThe organic layers were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-266e4b1777a9464ebbb59708489f5437
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987310B2
反応ノート
読み込み中…