Sodium hydride → HCID 67281141, Verbindung

HRID 1694718Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1694718
[H-].[Na+].[CH2:3]([NH:10][C:11]1[N:16]=[CH:15][C:14]([Br:17])=[CH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>CN(C=O)C>[Br:17][C:14]1[CH:15]=[N:16][C:11]([N:10]([CH2:3][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[S:19]([CH3:18])(=[O:21])=[O:20])=[N:12][CH:13]=1

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 31297Methanesulfonyl chlorideHCID 51391422-BENZYLAMINO-5-BROMOPYRIMIDINE

Produkt 1

HCID 67281141HCID 67281141, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Sodium hydride (0.1 g, 60% disp. in oil) was added to a stirred solution of benzyl-(5-bromo-pyrimidin-2-yl)-amine (0.55 g) in DMF (8 ml) at 0° C. After 30 min methanesulphonyl chloride (0.286 g) was added and the mixture stirred at RT for 2 h then partitioned between ethyl acetate and water. The organics were separated washed with water, dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with dichloromethane. Yield 0.41 g

Aufarbeitung

  1. customthen partitioned between ethyl acetate and water
  2. customThe organics were separated
  3. washwashed with water
  4. customdried
  5. customevaporated under reduced pressure
  6. customThe residue was purified by chromatography on silica eluting with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-8ac5083582b54a5881861183c061f556
Quelldatensatz
uspto-grants-2012_04
Patentnummer
US08158820B2

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