Hydrazine hydrate (1:1) → 2H,3H,4H,4aH,5H-indeno[1,2-c]pyridazin-3-one
반응식
O.[NH2:2][NH2:3].O=[C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]1[CH2:14][C:15]([OH:17])=O>C(O)C>[N:2]1[NH:3][C:15](=[O:17])[CH2:14][CH:6]2[CH2:7][C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:5]=12참가 물질
4
실험 절차
To a solution of 0.53 g (0.011 mol) of hydrazine hydrate dissolved in 25 mL ethanol was added 1.2 g (0.0089 mol) of the product from step B. The reaction mixture was refluxed for 18 hours, cooled to room temperature, concentrated under vacuum, added 100 mL H2O and extracted with ethyl acetate (3×50 mL), washed with brine (1×100 mL), dried over anhydrous magnesium sulfate, filtered and concentrated under vacuum to afford 1.0 g of a yellow solid.
후처리
- temperatureThe reaction mixture was refluxed for 18 hours
- concentrationconcentrated under vacuum
- additionadded 100 mL H2O
- extractionextracted with ethyl acetate (3×50 mL)
- washwashed with brine (1×100 mL)
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum
출처 및 근거
- ORD 기록
- ord-8fd80bfc373f4339b22f4772bf8ce9de
- 출처 데이터셋
- uspto-grants-1997_01
- 특허 번호
- US05591729
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