Hydrazine hydrate (1:1) → 4-Tert-butyl-5-hydroxymethylpyrazol-3-one
反応式
[C:1]([CH:5]1[C:9](O)=[CH:8][O:7][C:6]1=[O:11])([CH3:4])([CH3:3])[CH3:2].O.[NH2:13][NH2:14]>CCO>[C:1]([C:5]1[C:6](=[O:11])[N:13]=[N:14][C:9]=1[CH2:8][OH:7])([CH3:4])([CH3:3])[CH3:2]参加物
4
実験手順
3-tert-Butyl-4-hydroxy-2-furanone (6.6 g, 42 mmol) was dissolved in EtOH (75 mL) with hydrazine hydrate (6.6 mL, 0.21 mol) and was heated at reflux for 16h. The solvent was evaporated and the residue azeotroped with xylene ( 3×50 mL) to afford the title compound (7.2 g, 100%) as a colourless solid. mp 169-172° C. 1H NMR (360 MHz, d6-DMSO) δ1.26 (9H, s), 4.41 (2H, d, J=5.2 Hz), 4.97-5.01 (1H, m), 9.30 (1H, br s), 11.05 (1H, br s). MS (ES+) 171 (M+1).
後処理
- temperaturewas heated
- temperatureat reflux for 16h
- customThe solvent was evaporated
- customthe residue azeotroped with xylene ( 3×50 mL)
出典と根拠
- ORDレコード
- ord-fbf2da12e00044a4ad889c32a84ebbd7
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06355638B1
反応ノート
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