Hydrazine → 5,5-dimethyl-4,5,6,7-tetrahydro-1H-indazole
反応式
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]1参加物
4
実験手順
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).
後処理
- customresulted in an exothermic reaction
- concentrationthen concentrated
- customThe residue was triturated with petroleum ether
出典と根拠
- ORDレコード
- ord-bae5aa8a471048f6ad57d500cbe3fd6c
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
反応ノート
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