Water → HCID 22508608, Verbindung

HRID 984829Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 984829
Br[C:2]1[N:10]([CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[Cl:18])[C:9]2[C:8](=[O:19])[N:7]([CH2:20][C:21]3[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=3[C:23]#[N:24])[C:6](=[O:29])[N:5]([CH3:30])[C:4]=2[N:3]=1.[NH:31]1[CH2:37][CH2:36][CH2:35][CH2:34][CH:33]([NH2:38])[CH2:32]1.C(N(CC)CC)C.O>CS(C)=O.ClCCl>[NH2:38][CH:33]1[CH2:34][CH2:35][CH2:36][CH2:37][N:31]([C:2]2[N:10]([CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:18])[C:9]3[C:8](=[O:19])[N:7]([CH2:20][C:21]4[CH:28]=[CH:27][CH:26]=[CH:25][C:22]=4[C:23]#[N:24])[C:6](=[O:29])[N:5]([CH3:30])[C:4]=3[N:3]=2)[CH2:32]1

Komponenten

7

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 2756445Azepan-3-amineHCID 22508571HCID 22508571, Verbindung

Produkt 1

HCID 22508608HCID 22508608, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 679Dimethyl SulfoxideLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2-(8-Bromo-7-(2-chlorobenzyl)-3-methyl-2,6-dioxo-1,2,3,6-tetrahydropurin-1-ylmethyl)benzonitrile (75B) (250 mg, 0.5 mmol) and azepan-3-ylamine (294 mg, 2.5 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 HPLC (method A1, Rt=8.77 min.). Evaporation of the solvent afforded the title compound as an yellow oil.

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 HPLC (method A1, Rt=8.77 min.)
  5. customEvaporation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-f4625e3b97d54440990f05fef183ae97
Quelldatensatz
uspto-grants-2005_03
Patentnummer
US06869947B2

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