Hydrazine hydrate (1:1) → 4-Tert-butyl-5-hydroxymethylpyrazol-3-one
반응식
[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]참가 물질
4
실험 절차
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).
후처리
- temperaturewas heated
- temperatureat reflux for 16h
- customThe solvent was evaporated
- customthe residue azeotroped with xylene ( 3×50 mL)
출처 및 근거
- ORD 기록
- ord-fbf2da12e00044a4ad889c32a84ebbd7
- 출처 데이터셋
- uspto-grants-2002_03
- 특허 번호
- US06355638B1
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