Aniline → 7-(3-Chloropyridin-2-yl)-N-(phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

HRID 971219Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 971219
Cl[C:2]1[C:3]2[CH2:11][CH2:10][N:9]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][N:13]=3)[CH2:8][C:4]=2[N:5]=[CH:6][N:7]=1.[NH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>C(#N)C>[Cl:18][C:17]1[C:12]([N:9]2[CH2:10][CH2:11][C:3]3[C:2]([NH:19][C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)=[N:7][CH:6]=[N:5][C:4]=3[CH2:8]2)=[N:13][CH:14]=[CH:15][CH:16]=1

Komponenten

4

Edukt 2

HCID 6115AnilineHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

Produkt 1

HCID 120043447-(3-Chloropyridin-2-yl)-N-(phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amineAusbeute 32,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

4-Chloro-7-(3-chloro-pyridin-2-yl)-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine (150 mg, 0.54 mmol) was dissolved in acetonitrile (2 mL). To the mixture was added aniline (60 mg). The mixture was heated in a sealed tube at 180° C. for 30 minutes in a Personal Chemistry Microwave (Smith Creator). The solvent was removed under vacuum and the resulting orange residue was purified by flash chromatography over silica gel using a 0-100% ethyl acetate-hexane gradient to give the product as an off white solid (60 mg).

Aufarbeitung

  1. customThe solvent was removed under vacuum
  2. customthe resulting orange residue was purified by flash chromatography over silica gel using a 0-100% ethyl acetate-hexane gradient

Quellen und Nachweise

ORD-Eintrag
ord-516e1152c3be4900a1b97a1d5f54389c
Quelldatensatz
uspto-grants-2007_12
Patentnummer
US07312330B2

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