Acetate → HCID 16045655, Verbindung

HRID 1869085Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1869085
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 CH2Cl2/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-59440401be0a433e9a310298f19618c8
Quelldatensatz
uspto-grants-2009_12
Patentnummer
USRE041065E1

Notizen zur Reaktion

Wird geladen…