Hydrochloric Acid → (3,5-Dibromothiophen-2-yl)-oxo-acetic acid
反応式
C([O:3][C:4](=[O:14])[C:5]([C:7]1[S:8][C:9]([Br:13])=[CH:10][C:11]=1[Br:12])=[O:6])C.Cl>CC(C)=O>[Br:12][C:11]1[CH:10]=[C:9]([Br:13])[S:8][C:7]=1[C:5](=[O:6])[C:4]([OH:14])=[O:3]参加物
4
実験手順
(3,5-Dibromothiophen-2-yl)-oxo-acetic acid ethyl ester (513 mg, 1.50 mmol) was dissolved in 25 ml acetone and treated with 15 ml 8 N HCl at reflux for a total of 4 hours. The reaction mixture was concentrated in vacuo, poured into 50 ml water, and extracted into 100 ml of dichloromethane. The organic layer was dried over Na2SO4 and concentrated in vacuo to yield (3,5-dibromothiophen-2-yl)-oxo-acetic acid (467 mg, 99%). MS (M+H)+: 314.84; 1H NMR (300 MHz, DMSO-d6) δ7.64 (1H, s).
後処理
- temperatureat reflux for a total of 4 hours
- concentrationThe reaction mixture was concentrated in vacuo
- additionpoured into 50 ml water
- extractionextracted into 100 ml of dichloromethane
- dry with materialThe organic layer was dried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-1bac93bc577a4939b2af6f105182e7bd
- 出典データセット
- uspto-grants-2003_09
- 特許番号
- US06613786B2
反応ノート
読み込み中…