Hydrazine → 5,5-dimethyl-4,5,6,7-tetrahydro-1H-indazole
반응식
O/[CH:2]=[C:3]1\[C:4](=O)[CH2:5][CH2:6][C:7]([CH3:10])([CH3:9])[CH2:8]\1.[NH2:12][NH2:13]>CO>[CH3:9][C:7]1([CH3:10])[CH2:6][CH2:5][C:4]2[NH:13][N:12]=[CH:2][C:3]=2[CH2:8]1참가 물질
4
실험 절차
In a 100 ml round-bottomed flask, 2-[1-hydroxy-meth-(Z)-ylidene]-4,4-dimethyl-cyclohexanone (1.30 g, 8.43 mmol) was dissolved in methanol (8.5 ml). Hydrazine (0.27 ml, 8.43 mmol) was added very slowly which resulted in an exothermic reaction. The reaction mixture was stirred at room temperature for 50 min then concentrated. The residue was triturated with petroleum ether to afford 1.05 g (83%) of 5,5-dimethyl-4,5,6,7-tetrahydro-1H-indazole as a light brown solid. 1H NMR (CDCl3, 300 MHz): δ (ppm) 7.28 (s, 1H), 2.67 (t, J=6.6 Hz, 2H), 2.32 (s, 2H), 1.60 (t, J=6.6 Hz, 2H), 0.99 (s, 6H).
후처리
- customresulted in an exothermic reaction
- concentrationthen concentrated
- customThe residue was triturated with petroleum ether
출처 및 근거
- ORD 기록
- ord-bae5aa8a471048f6ad57d500cbe3fd6c
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08658646B2
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