Hydrazine hydrate (1:1) → HCID 3682963、化合物
反応式
C([O:3][C:4](=O)[CH2:5][N:6]1[CH:10]=[CH:9][C:8]([CH3:11])=[N:7]1)C.O.[NH2:14][NH2:15]>C(O)C>[CH3:11][C:8]1[CH:9]=[CH:10][N:6]([CH2:5][C:4]([NH:14][NH2:15])=[O:3])[N:7]=1参加物
4
実験手順
As described for example 112a, (3-methyl-pyrazol-1-yl)-acetic acid ethyl ester in ethanol was reacted with hydrazine hydrate (2 equivalents) and the resulting mixture was heated under reflux for 4 h. The mixture was then cooled to rt and the precipitated product was filtered off and crystallized from ethanol. The title compound (>95% purity) was obtained as a white solid (yield: 68%). 1H-NMR (300 MHz, DMSO): δ=2.12 (s, 3H), 4.29 (s, 2H), 4.60 (s, 2H), 6.00 (d, J=2 Hz, 1H), 7.55 (d, J=2 Hz, 1H), 9.26 (s, 1H).
後処理
- temperaturethe resulting mixture was heated
- temperatureunder reflux for 4 h
- filtrationthe precipitated product was filtered off
- customcrystallized from ethanol
出典と根拠
- ORDレコード
- ord-6e5b8b40a88e48a4b53eaef1fa584e19
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07507729B2
反応ノート
読み込み中…