Hydrochloric Acid → (3,5-Dibromothiophen-2-yl)-oxo-acetic acid
반응식
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]참가 물질
4
실험 절차
(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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-1bac93bc577a4939b2af6f105182e7bd
- 출처 데이터셋
- uspto-grants-2003_09
- 특허 번호
- US06613786B2
반응 노트
불러오는 중…