Ethyl benzoylacetate → HCID 178469958, 화합물

HRID 386648

반응식

HRID 386648 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 178469958HCID 178469958, 화합물수율 61%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-d0ac4a62de4d465aa9805715d06346f8
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372851B2

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