Hydrazine hydrate (1:1) → HCID 68406318、化合物
反応式
C([O:3][C:4](=O)[CH2:5][C:6]1[CH:7]=[N:8][C:9]([CH3:12])=[CH:10][CH:11]=1)C.O.[NH2:15][NH2:16]>C(O)CCC>[CH3:12][C:9]1[N:8]=[CH:7][C:6]([CH2:5][C:4]([NH:15][NH2:16])=[O:3])=[CH:11][CH:10]=1参加物
4
実験手順
As described for example 112a, (6-methyl-pyridin-3-yl)-acetic acid ethyl ester in butanol was reacted with hydrazine hydrate (2 equivalents) and the resulting mixture was then heated under reflux for 20 h. Evaporation of all volatiles and crystallization from n-butanol and toluene afforded the title compound as a white solid (yield: 72%). 1H-NMR (300 MHz, DMSO): δ=2.42 (s, 3H), 3.32 (s, 2H), 4.21 (s, 2H), 7.17 (d, J=8 Hz, 1H), 7.53 (dd, J=2 Hz, J=8 Hz, 1H), 8.30 (d, J=2 Hz, 1H), 9.23 (s, 1H).
後処理
- temperaturethe resulting mixture was then heated
- temperatureunder reflux for 20 h
- customEvaporation of all volatiles and crystallization from n-butanol and toluene
出典と根拠
- ORDレコード
- ord-fc87e9f8a2654a88b7073a18c13fa270
- 出典データセット
- uspto-grants-2009_03
- 特許番号
- US07507729B2
反応ノート
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