Lithium hydride → 3-Chloro-6,7-dihydro-[1,4]dioxino[2,3-c]pyridazine
반응식
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:12])=[CH:6][C:7]=1[O:8][CH2:9][CH2:10][OH:11].[H-].[Li+]>O1CCOCC1>[Cl:12][C:5]1[N:4]=[N:3][C:2]2[O:11][CH2:10][CH2:9][O:8][C:7]=2[CH:6]=1참가 물질
4
실험 절차
A solution of 2-[(3,6-dichloro-4-pyridazinyl)oxy]ethanol containing some bromo-derivative (15.46 g; 0.0703 mol) in dry 1,4-dioxane (1.2 L) was treated with lithium hydride (2.3 g; 0.28 mol) in portions and stirred at room temperature for 1 hour under argon, then heated at 110° C. overnight. The reaction mixture was quenched with wet 1,4-dioxane, then iced-water. The solution was evaporated to half volume, taken to pH 8 with 5M hydrochloric acid and evaporated to dryness. Water was added and the residue was extracted 5× with chloroform, dried (sodium sulphate) and evaporated to afford a white solid (12.4 g, ca. 77%) (containing ca. 15% of a bromo species).
후처리
- temperatureheated at 110° C. overnight
- customThe reaction mixture was quenched with wet 1,4-dioxane
- customThe solution was evaporated to half volume
- customevaporated to dryness
- additionWater was added
- extractionthe residue was extracted 5× with chloroform
- dry with materialdried (sodium sulphate)
- customevaporated
- customto afford
출처 및 근거
- ORD 기록
- ord-ce358187d37146d6ae74d6a3c5e65e0d
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07732460B2
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