Ammonium Hydroxide → 1,5-diethyl-1H-pyrazole-3-carboxamide
反応式
[CH2:1]([N:3]1[C:7]([CH2:8][CH3:9])=[CH:6][C:5]([C:10]([O:12]CC)=O)=[N:4]1)[CH3:2].[OH-].[NH4+:16]>>[CH2:1]([N:3]1[C:7]([CH2:8][CH3:9])=[CH:6][C:5]([C:10]([NH2:16])=[O:12])=[N:4]1)[CH3:2]参加物
3
実験手順
A mixture of ethyl 1,5-diethyl-1H-pyrazole-3-carboxylate (29.4 g, 0.50 mol) and ammonium hydroxide (150 mL of 30%) was stirred overnight at ambient temperature. An analysis by thin layer chromatography (TLC) indicated the reaction was incomplete. The reaction was then heated for 14 hours at 125° C. in a pressure vessel, allowed to cool to ambient temperature, and cooled to 0° C. A precipitate formed, was isolated by filtration, and washed with cold hexanes to provide 8.3 g of 1,5-diethyl-1H-pyrazole-3-carboxamide as a white solid, mp 129-131° C.
後処理
- temperatureThe reaction was then heated for 14 hours at 125° C. in a pressure vessel
- temperatureto cool to ambient temperature
- temperaturecooled to 0° C
- customA precipitate formed
- customwas isolated by filtration
- washwashed with cold hexanes
出典と根拠
- ORDレコード
- ord-22aa986d65324142990d2f6325dd6a24
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07544697B2
反応ノート
読み込み中…