Ethyl benzoylacetate → HCID 178469958、化合物

HRID 386648

反応式

HRID 386648 の反応式
[NH2:1][C:2]1[NH:6][N:5]=[CH:4][C:3]=1[C:7]([O:9][CH2:10][CH3:11])=[O:8].O=[C:13]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:14][C:15](OCC)=[O:16]>C(O)(=O)C>[OH:16][C:15]1[N:6]2[N:5]=[CH:4][C:3]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[C:2]2[N:1]=[C:13]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:14]=1

参加物

4

反応物 2

HCID 7170Ethyl benzoylacetateHCID 81472ethyl 3-amino-1H-pyrazole-4-carboxylate

生成物 1

HCID 178469958HCID 178469958、化合物収率 61%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Commercially available ethyl 5-amino-1H-pyrazole-4-carboxylate (5.0 g, 32 mmol) was taken into glacial acetic acid (3.2 mL) followed by addition of ethyl 3-oxo-3-phenylpropanoate (6.1 mL, 35 mmol) and the mixture was refluxed for 12 h. The mixture was allowed to cool to room temperature and concentrated in vacuo. The crude solid was recrystallized (ethanol) and collected to yield 3.1 g (61%) of crystalline ethyl 7-hydroxy-5-phenylpyrazolo[1,5-a]pyrimidine-3-carboxylate. 1H NMR (400 MHz, d6-DMSO): 11.75 (s, 1H), 8.28 (s, 1H), 7.80 (m, 2H), 7.61 (m, 3H), 6.28 (s, 1H), 4.31 (q, 2H), 1.34 (t, 3H).

後処理

  1. temperaturethe mixture was refluxed for 12 h
  2. concentrationconcentrated in vacuo
  3. customThe crude solid was recrystallized (ethanol)
  4. customcollected

出典と根拠

ORDレコード
ord-d0ac4a62de4d465aa9805715d06346f8
出典データセット
uspto-grants-2013_02
特許番号
US08372851B2

関連ノート

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