Water → 8-(3-Aminoazepan-1-yl)-7-benzyl-3-methyl-1-(2-oxo-2-phenylethyl)-3,7-dihydropurine-2,6-dione

HRID 984832

Reaktionsgleichung

Reaktionsgleichung von HRID 984832
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[N:14]([CH2:18][C:19](=[O:26])[C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[C:13](=[O:27])[N:12]([CH3:28])[C:11]=2[N:10]=[C:9]1Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH:30]1[CH2:36][CH2:35][CH2:34][CH2:33][CH:32]([NH2:37])[CH2:31]1.C(N(CC)CC)C.O>CS(C)=O.ClCCl>[NH2:37][CH:32]1[CH2:33][CH2:34][CH2:35][CH2:36][N:30]([C:9]2[N:8]([CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)[C:16]3[C:15](=[O:17])[N:14]([CH2:18][C:19](=[O:26])[C:20]4[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=4)[C:13](=[O:27])[N:12]([CH3:28])[C:11]=3[N:10]=2)[CH2:31]1

Komponenten

7

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 225085767-Benzyl-8-bromo-3-methyl-1-(2-oxo-2-phenylethyl)-3,7-dihydropurine-2,6-dione

Produkt 1

HCID 225086468-(3-Aminoazepan-1-yl)-7-benzyl-3-methyl-1-(2-oxo-2-phenylethyl)-3,7-dihydropurine-2,6-dione

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

7-Benzyl-8-bromo-3-methyl-1-(2-oxo-2-phenylethyl)-3,7-dihydropurine-2,6-dione (77B) (227 mg, 0.5 mmol) and azepan-3-ylamine (342 mg, 3 mmol), and triethylamine (0.35 ml, 2.5 mmol) were dissolved in 20 ml of DMSO and the mixture was subjected to microwaves (method F, 100° C., 300 W) for five hours. To the reaction mixture was added 100 ml of water and 100 ml of dichloromethane, and the organic layer was separated and dried over sodium sulfate. The solvents were evaporated and the crude product was purified by preparative

Aufarbeitung

  1. customthe organic layer was separated
  2. dry with materialdried over sodium sulfate
  3. customThe solvents were evaporated
  4. customthe crude product was purified by preparative

Quellen und Nachweise

ORD-Eintrag
ord-ab312c483e4848ddaa7edabeafe33b88
Quelldatensatz
uspto-grants-2005_03
Patentnummer
US06869947B2

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