9-benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione → 2-[(3-Chlorophenyl)methyl]-7-(2,2-dimethylbutanoyl)-9-hydroxy-3,4-dihydropyrido[1,2-a]pyrazine-1,8-dione

HRID 1349500Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1349500
C([O:8][C:9]1[C:10](=[O:35])[C:11]([C:28](=[O:34])[C:29]([CH3:33])([CH3:32])[CH2:30][CH3:31])=[CH:12][N:13]2[CH2:18][CH2:17][N:16]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=3)[C:15](=[O:27])[C:14]=12)C1C=CC=CC=1>FC(F)(F)C(O)=O>[Cl:26][C:22]1[CH:21]=[C:20]([CH:25]=[CH:24][CH:23]=1)[CH2:19][N:16]1[CH2:17][CH2:18][N:13]2[CH:12]=[C:11]([C:28](=[O:34])[C:29]([CH3:32])([CH3:33])[CH2:30][CH3:31])[C:10](=[O:35])[C:9]([OH:8])=[C:14]2[C:15]1=[O:27]

Komponenten

3

Edukt 1

HCID 230774849-benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione

Produkt 1

HCID 546833552-[(3-Chlorophenyl)methyl]-7-(2,2-dimethylbutanoyl)-9-hydroxy-3,4-dihydropyrido[1,2-a]pyrazine-1,8-dioneAusbeute 71,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

9-Benzyloxy-2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione (55 mg) was dissolved in trifluoroacetic acid (0.5 ml) and the mixture was stirred at room temperature for 30 min. The solvent was evaporated and toluene was added, and the mixture was concentrated, which operations were performed twice. Crystallization from chloroform-diisopropyl ether gave 2-(3-chlorobenzyl)-7-(2,2-dimethylbutyryl)-9-hydroxy-3,4-dihydro-2H-pyrido[1,2-a]pyrazine-1,8-dione (32 mg).

Aufarbeitung

  1. customThe solvent was evaporated
  2. additiontoluene was added
  3. concentrationthe mixture was concentrated
  4. customCrystallization from chloroform-diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-1bfa144d9ff14d4d84e815ae5f37897e
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07211572B2

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