Acetate → HCID 16045655, Verbindung

HRID 1288876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1288876
Cl.Cl[CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18]Cl)[N:12]=[CH:11][N:10]=[C:9]2[NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([C:27]#[CH:28])[CH:22]=1.[C:29]([O-:32])(=[O:31])[CH3:30]>CN(C=O)C>[C:29]([O:32][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][C:15]=1[O:16][CH2:17][CH2:18][O:32][C:29](=[O:31])[CH3:30])[N:12]=[CH:11][N:10]=[C:9]2[NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([C:27]#[CH:28])[CH:22]=1)(=[O:31])[CH3:30]

Komponenten

4

Edukt 2

HCID 175AcetateHCID 189250636,7-Bis(2-chloroethoxy)-N-(3-ethynylphenyl)quinazolin-4-amine--hydrogen chloride (1/1)

Produkt 1

HCID 16045655HCID 16045655, VerbindungAusbeute 135,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The title product of Example 29 (200 mg, 0.456 mmol) was treated with cesuim acetate (1.75 g, 9.12 mmol) in DMF (3 mL) at 120° C. under an atmosphere of N2 for 16 hours. The reaction mixture was partitioned between brine and CHCl3, and the organic extract was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford an oil (277 mg) which was recrystallized from CH2 Cl2 /hexane. (184 mg; 90%; M.P. 137°-138° C.; LC-MS: 450 (MH+); anal. RP18-HPLC RT: 4.64 min.).

Aufarbeitung

  1. customThe reaction mixture was partitioned between brine and CHCl3
  2. extractionthe organic extract
  3. washwas washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-3f950a51aec74cba833b56e039d844c2
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05747498

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