Toluene → 2-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine

HRID 66002Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 66002
Cl[C:2]1[N:3]=[CH:4][C:5]2[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=2[N:7]=1.[CH2:20]([N:27]1[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C1(C)C=CC=CC=1>C(Cl)(Cl)Cl.O>[CH2:20]([N:27]1[CH2:32][CH2:31][N:30]([C:2]2[N:3]=[CH:4][C:5]3[C:11](=[O:12])[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][N:8]([CH2:18][CH3:19])[C:6]=3[N:7]=2)[CH2:29][CH2:28]1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1

Komponenten

6

Edukt 3

HCID 1140TolueneHCID 759941-BenzylpiperazineHCID 122668052-Chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine

Produkt 1

HCID 122668082-(4'-Benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidineAusbeute 90 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

As described in Example VI, a mixture of 5.6 g. of 2-chloro-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydropyrido(2,3-d)pyrimidine, 7.04 g. of N-benzylpiperazine and 80 cm3 of toluene is heated under reflux for 2 hours. After cooling, the mass is diluted with 100 cm3 of chloroform and is taken up in 200 cm3 of water. After washing the organic phase with water, the reaction product is isolated as described in the Example mentioned. It is recrystallised from isopropanol. 7.6 g. (90%) of 2-(4'-benzyl-piperazino)-5-oxo-6-carbethoxy-8-ethyl-5,8-dihydro-pyrido(2,3-d)pyrimidine are obtained; melting point 152° C.

Aufarbeitung

  1. additiona mixture of 5.6 g
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. washAfter washing the organic phase with water
  5. customthe reaction product is isolated
  6. customIt is recrystallised from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-fa47c2ad0e9e443182fecb169b01b9ea
Quelldatensatz
uspto-grants-1978_12
Patentnummer
US04129737

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