Ethyl 2,4-dioxovalerate → HCID 178427252、化合物
反応式
[NH2:1][C:2]1[CH:3]=[C:4]([OH:7])[NH:5][N:6]=1.C[O-].[Na+].C([O:13][C:14](=[O:21])[C:15](=O)[CH2:16][C:17](=O)[CH3:18])C>CO>[OH:7][C:4]1[C:3]2[C:2](=[N:1][C:15]([C:14]([OH:21])=[O:13])=[CH:16][C:17]=2[CH3:18])[NH:6][N:5]=1参加物
5
実験手順
5-Amino-2H-pyrazol-3-ol (3.1 g, 31.6 mmol) were suspended in 100 ml of methanol. Then sodium methoxide (5.1 g, 95 mmol) and 2,4-dioxopentanoic acid ethyl ester (5 g, 31.6 mmol) were added, and the mixture was heated up under reflux for 12 h. The solvent was removed in a rotary evaporator, water was added to the residue, the precipitate was filtered off with suction, and the filtrate was adjusted to pH 6 with dilute hydrochloric acid. The precipitated product (both precipitates) was filtered off with suction and dried. Yield: 4.9 g (70%), M+H+: 194.09.
後処理
- temperaturethe mixture was heated up
- temperatureunder reflux for 12 h
- customThe solvent was removed in a rotary evaporator, water
- additionwas added to the residue
- filtrationthe precipitate was filtered off with suction
- customThe precipitated product (both precipitates)
- filtrationwas filtered off with suction
- customdried
出典と根拠
- ORDレコード
- ord-914644e5cbc34774a7cd954f93d41aff
- 出典データセット
- uspto-grants-2009_05
- 特許番号
- US07528155B2
反応ノート
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