Acetonitrile → HCID 12004101, Verbindung

HRID 971258Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 971258
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:28]=[C:27]2[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]2[C:29](=[O:31])[CH3:30])=[CH:22][CH:21]=1.C(#N)C.C(=O)(O)[O-].[Na+]>CCOC(C)=O>[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:28]=[C:27]5[C:23]([C:24]([CH3:33])([CH3:32])[CH2:25][N:26]5[C:29](=[O:31])[CH3:30])=[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

6

Edukt 4

HCID 6342AcetonitrileHCID 516892Sodium BicarbonateHCID 218651761-(6-Amino-3,3-dimethylindolin-1-yl)ethanoneHCID 590214784-Chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

Produkt 1

HCID 12004101HCID 12004101, VerbindungAusbeute 79,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
180 °C

Versuchsvorschrift

A mixture of 4-chloro-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine (40 mg, 0.14 mmol), 1-(6-amino-3,3-dimethylindolin-1-yl)ethanone (60 mg, 0.29 mmol), and acetonitrile (3 mL) was heated in a sealed tube via microwave at 180° C. for 60 min. The mixture was treated with EtOAc (50 mL) and saturated aqueous sodium bicarbonate. The organic layer was separated and washed with brine, dried (Na2SO4), and evaporated. The residue was purified by flash chromatography over silica gel to give an off-white solid (50 mg).

Aufarbeitung

  1. customThe organic layer was separated
  2. washwashed with brine
  3. dry with materialdried (Na2SO4)
  4. customevaporated
  5. customThe residue was purified by flash chromatography over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-412e5b5c6c0e4f23b1cad564a8d9fc7b
Quelldatensatz
uspto-grants-2007_12
Patentnummer
US07312330B2

Notizen zur Reaktion

Wird geladen…