Piperazine → HCID 68843659, Verbindung

HRID 1517400Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1517400
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]([NH:10][C:11]1[N:12]=[C:13](C2N=CNN=2)[C:14]2[N:20]=[C:19]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[C:23]([O:29][CH3:30])[CH:22]=3)[CH:18]=[CH:17][C:15]=2[N:16]=1)(=[O:9])[CH3:8]>O1CCOCC1>[C:7]([NH:10][C:11]1[N:12]=[C:13]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[C:14]2[N:20]=[C:19]([C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[C:23]([O:29][CH3:30])[CH:22]=3)[CH:18]=[CH:17][C:15]=2[N:16]=1)(=[O:9])[CH3:8]

Komponenten

4

Edukt 2

HCID 4837PiperazineHCID 178488517HCID 178488517, Verbindung

Produkt 1

HCID 68843659HCID 68843659, VerbindungAusbeute 79 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Piperazine (430 mg, 5 mmole) was added to a stirred suspension of 2-acetamido-6-(3,4-dimethoxyphenyl)-4-(1,2,4-triazolyl)pyrido[3,2-d]pyrimidine (977 mg, 2.5 mmole) in dioxane (70 ml). The reaction mixture was refluxed for 16 hours. The precipitate was filtered off and washed with a small amount of dioxane. The filtrate was evaporated to dryness and the residue washed with diethyl ether. Both fractions (the precipitate and the washed filtrate) were combined, resulting in the pure title compound (805 mg, yield 79%) which was characterized by its mass spectrum as follows: MS (m/z): 409 ([M+H]+, 100).

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 16 hours
  2. filtrationThe precipitate was filtered off
  3. washwashed with a small amount of dioxane
  4. customThe filtrate was evaporated to dryness
  5. washthe residue washed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-21f6ffaa6cf846318ced0ce1dd2c8f18
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08232278B2

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