Bromine → 6-Isopropyl-3-pyridazinone
반응식
[CH:1]([C:4]1[CH2:5][CH2:6][C:7](=[O:10])[NH:8][N:9]=1)([CH3:3])[CH3:2].BrBr>C(O)(=O)C>[CH:1]([C:4]1[CH:5]=[CH:6][C:7](=[O:10])[NH:8][N:9]=1)([CH3:3])[CH3:2]참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
4,5-Dihydro-6-isopropyl-3 (2H)-pyridazinone (3.10 g) was dissolved in acetic acid (30.0 ml), and bromine (3.50 g, 22.0 mmol) was added dropwise to the solution over 10 minutes under heating at 100° C. with stirring. After the reaction solution was heated for 1 hour under reflux, the acetic acid was distilled away under reduced pressure, and water (100 ml) was added to the residues which were then extracted 5 times with ethyl acetate. The extracts were combined, dried over anhydrous magnesium sulfate and concentrated to give a crude product of 6-isopropyl-3 (2H)-pyridazinone. The yield was 3.30 g.
후처리
- temperatureAfter the reaction solution was heated for 1 hour
- temperatureunder reflux
- distillationthe acetic acid was distilled away under reduced pressure, and water (100 ml)
- additionwas added to the residues which
- extractionwere then extracted 5 times with ethyl acetate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-36e88ef656cd4951b6257773619e1d31
- 출처 데이터셋
- uspto-grants-2010_10
- 특허 번호
- US07816526B2
반응 노트
불러오는 중…