Acetic Acid → 3,5-Dibromopyridine-2-carboxylic acid
반응식
C([C:3]1[C:8]([Br:9])=[CH:7][C:6]([Br:10])=C[N:4]=1)#N.[C:11]([OH:14])(=[O:13])[CH3:12].S(=O)(=O)(O)O>O>[Br:10][C:6]1[C:12]([C:11]([OH:14])=[O:13])=[N:4][CH:3]=[C:8]([Br:9])[CH:7]=1참가 물질
5
반응 조건
- 온도
- 140 °C
실험 절차
2-Cyano-3,5-dibromopyridine (prepared in the above (2)) 3.27 g is added to a mixture of acetic acid 14 ml, sulfuric acid 14 ml and water 14 ml, and the mixture is refluxed at 140° C. for 4 hours. The reaction mixture is cooled and water is added thereto. The resulting precipitate is filtered and washed with water. The precipitate is dissolved in ether, washed and dried. The solvent is removed in vacuo and crystallized from a mixture of ether and hexane to give 3,5-dibromopyridine-2-carboxylic acid. mp 170–171° C.
후처리
- temperatureThe reaction mixture is cooled
- filtrationThe resulting precipitate is filtered
- washwashed with water
- dissolutionThe precipitate is dissolved in ether
- washwashed
- customdried
- customThe solvent is removed in vacuo
- customcrystallized from a mixture of ether and hexane
출처 및 근거
- ORD 기록
- ord-c8f7d0c165bd4808a2e405c0309f4b35
- 출처 데이터셋
- uspto-grants-2007_05
- 특허 번호
- US07220736B2
반응 노트
불러오는 중…