Hydrochloric Acid → 7-(3-Chloropyridin-2-yl)-5,6,7,8-tetrahydro-n-(1,3,3-trimethylindolin-6-yl)pyrido[3,4-d]pyrimidin-4-amine

HRID 971260Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 971260
[Cl:1][C:2]1[C:3]([N:8]2[CH2:17][CH2:16][C:15]3[C:14]([NH:18][C:19]4[CH:27]=[C:26]5[C:22]([C:23]([CH3:29])([CH3:28])[CH2:24][NH:25]5)=[CH:21][CH:20]=4)=[N:13][CH:12]=[N:11][C:10]=3[CH2:9]2)=[N:4][CH:5]=[CH:6][CH:7]=1.Cl.[C:31]([O-])([O-])=O.[K+].[K+].CI>CN(C=O)C.O>[Cl:1][C:2]1[C:3]([N:8]2[CH2:17][CH2:16][C:15]3[C:14]([NH:18][C:19]4[CH:27]=[C:26]5[C:22]([C:23]([CH3:29])([CH3:28])[CH2:24][N:25]5[CH3:31])=[CH:21][CH:20]=4)=[N:13][CH:12]=[N:11][C:10]=3[CH2:9]2)=[N:4][CH:5]=[CH:6][CH:7]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 120041027-(3-Chloropyridin-2-yl)-5,6,7,8-tetrahydro-n-(3,3-dimethylindolin-6-yl)pyrido[3,4-d]pyrimidin-4-amine

Produkt 1

HCID 120041037-(3-Chloropyridin-2-yl)-5,6,7,8-tetrahydro-n-(1,3,3-trimethylindolin-6-yl)pyrido[3,4-d]pyrimidin-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a stirred solution of compound of Example 69 hydrogen chloride (20 mg) in DMF (5 mL) was added K2CO3 (50 mg), followed by MeI (50 μL). The mixture was stirred at room temperature for 2 h, and then treated with water, extracted with EtOAc (50 mL). The organic layer was separated, washed with brine, dried (Na2SO4), and evaporated. The residue was purified by flash chromatography over silica ghel to give a light yellow solid (10 mg).

Aufarbeitung

  1. extractionextracted with EtOAc (50 mL)
  2. customThe organic layer was separated
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated
  6. customThe residue was purified by flash chromatography over silica ghel

Quellen und Nachweise

ORD-Eintrag
ord-8af38c3f5dad42db993a610dd6212e26
Quelldatensatz
uspto-grants-2007_12
Patentnummer
US07312330B2

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