Ammonia → HCID 13359100, Verbindung

HRID 65994

Reaktionsgleichung

Reaktionsgleichung von HRID 65994
[NH2:1][C:2]1[CH:3]=[CH:4][N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:6]=1.C([O:15][C:16](=O)[CH2:17][C:18](=O)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)C.N>O>[C:7]1([N:5]2[N:6]3[C:16](=[O:15])[CH:17]=[C:18]([C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[N:1]=[C:2]3[CH:3]=[CH:4]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 7170Ethyl benzoylacetateHCID 5943201-phenyl-1H-pyrazol-3-amine

Produkt 1

HCID 13359100HCID 13359100, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 10 g. of 5-amino-2-phenylpyrazole (0.063 mol.),12.1 g. of benzoylacetic acid ethyl ester (0.063 mol.) and 50 g. of polyphosphoric acid is heated at 110°-120° with stirring for 90 minutes. After cooling, 200 ml. of water and then concentrated aqueous ammonia is added under external cooling to adjust the mixture to pH 9. The collected 1,5-diphenylpyrazolo[1,5-a]pyrimidin-7(1H)-one is washed with water and dried at 70°, yield: 17 g. (94%); m.p. 194°-200°. A sample, recrystallized from absolute ethanol, melts at 205°-207°.

Aufarbeitung

  1. additionA mixture of 10 g
  2. temperatureAfter cooling
  3. temperatureunder external cooling
  4. washThe collected 1,5-diphenylpyrazolo[1,5-a]pyrimidin-7(1H)-one is washed with water
  5. customdried at 70°
  6. customA sample, recrystallized from absolute ethanol, melts at 205°-207°

Quellen und Nachweise

ORD-Eintrag
ord-c89aecfb2a7e473eb71eb9b49edc3698
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04129738

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