Methyl iodide → 9-Butyl-2-chloro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

HRID 2111356

Reaktionsgleichung

Reaktionsgleichung von HRID 2111356
[CH2:1]([N:5]1[CH2:11][CH2:10][C:9](=[O:12])[NH:8][C:7]2[CH:13]=[N:14][C:15]([Cl:17])=[N:16][C:6]1=2)[CH2:2][CH2:3][CH3:4].[CH3:18]N(C)C(=O)C.IC.[H-].[Na+]>O>[CH2:1]([N:5]1[CH2:11][CH2:10][C:9](=[O:12])[N:8]([CH3:18])[C:7]2[CH:13]=[N:14][C:15]([Cl:17])=[N:16][C:6]1=2)[CH2:2][CH2:3][CH3:4]

Komponenten

6

Edukt 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 31374DimethylacetamideHCID 866234189-Butyl-2-chloro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

Produkt 1

HCID 866234199-Butyl-2-chloro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a mixture of 0.102 g (0.0004 mole) of 9-butyl-2-chloro-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VI-44), 1 mL of N,N-dimethylacetamide and 0.037 mL (0.0006 mole) of iodomethane at 0 degrees was added 0.024 g (0.0006 mole) of 60% sodium hydride in oil. The mixture was stirred at ambient temperature for 1 hour, then 20 mL of water was added. The precipitate was collected by filtration to give 0.094 g of 9-butyl-2-chloro-5-methyl-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-44) as an yellow solid.

Aufarbeitung

  1. filtrationThe precipitate was collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-15faebc5b8e446cea5282e3d4f885a99
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07517873B2

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