Acetone → 6-(1-Piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

HRID 1074392Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1074392
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][CH:13]=[CH:14][N:4]2[N:3]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1.CC(C)=O>C(Cl)Cl>[N:15]1([C:2]2[C:11]3[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[C:5]3=[N:12][CH:13]=[CH:14][N:4]3[N:3]=2)[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 8082PiperidineHCID 131789756-Chloro-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

Produkt 1

HCID 131789776-(1-Piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture was prepared by adding 15 g of 6-chloro-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine to 30.5 g of piperidine and the mixture was heated at reflux for 72 hours. The mixture was subjected to preparative liquid chromatography using 15% acetone in methylene chloride to separate the desired product from the impurities. The appropriate fractions from the chromatography were combined and the solvent was evaporated under reduced pressure. The resulting solid was collected by filtration and dried to give 6-(1-piperidinyl)-7,8,9,10-tetrahydroimidazo[2,1-a]phthalazine melting at about 95° C. This compound has the following structural formula ##STR2##

Aufarbeitung

  1. customA mixture was prepared
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 72 hours
  4. customto separate the desired product from the impurities
  5. customthe solvent was evaporated under reduced pressure
  6. filtrationThe resulting solid was collected by filtration
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-d33de4cc8e604d8ea697708b4ad14219
Quelldatensatz
uspto-grants-1983_07
Patentnummer
US04391807

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