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Acetic Acid → n-(3-{[3-(2-Chloro-phenyl)-6-fluoro-4-oxo-3,4-dihydro-quinazolin-2-ylmethyl]-amino}-phenyl)-acetamide

HRID 1169264
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1169264
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([F:19])[CH:15]=2)[N:10]=[C:9]1C=O.[CH:22]1[CH:27]=[C:26]([NH2:28])[CH:25]=[C:24](CC(N)=O)[CH:23]=1.Cl.[CH2:34]([N:36](CC)CC)C.[C:41]([OH:44])(=O)[CH3:42].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:17](=[O:18])[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([F:19])[CH:15]=2)[N:10]=[C:9]1[CH2:34][NH:36][C:24]1[CH:25]=[C:26]([NH:28][C:41](=[O:44])[CH3:42])[CH:27]=[CH:22][CH:23]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 176Acetic AcidHCID 8471TriethylamineHCID 108822Acetamide, N-(3-aminophenyl)-, hydrochloride (1:?)HCID 5049666Sodium triacetoxyborohydrideHCID 106858093-(2-Chlorophenyl)-6-fluoro-3,4-dihydroquinazolin-4-one-2-carboxaldehyde

Produkt 1

HCID 10173540
n-(3-{[3-(2-Chloro-phenyl)-6-fluoro-4-oxo-3,4-dihydro-quinazolin-2-ylmethyl]-amino}-phenyl)-acetamide
Ausbeute 24,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A mixture of 3-(2-chloro-phenyl)-6-fluoro-3,4-dihydro-quinazolin-4-one-2-carboxaldehyde (0.20 g, 0.66 mmol), 3-aminoacetanilide hydrochloride (0.062 g, 0.33 mmol), triethylamine (0.092 mL, 0.66 mmol), and acetic acid (0.19 mL, 3.3 mmol) in dichloroethane (10 mL) was chilled to 0° C. and sodium triacetoxyborohydride (0.350 g, 1.65 mmol) was added. The reaction was stirred for 1 hour at 0° C. and then allowed to warm to ambient temperature and stirred 16 hours. The reaction was quenched by addition of saturated aqueous bicarbonate and continued stirring for 30 minutes. The phases were separated and the aqueous layer was extracted with methylene chloride. The combined organic phase was washed with brine, dried over magnesium sulfate and concentrated. The residue triturated with 50% isopropyl ether/hexane to afford 0.035 g (24%) of N-(3-{[3-(2-Chloro-phenyl)-6-fluoro-4-oxo-3,4-dihydro-quinazolin-2-ylmethyl]-amino}-phenyl)-acetamide as a yellow solid which had: 1H NMR δ 7.92 (dd, J=3, 8 Hz, 1H), 7.86 (dd, J=5, 9 Hz, 1H), 7.67-7.64 (m, 1H), 7.56-7.48 (m, 4H), 7.40 (dd, J=2, 7 Hz, 1H), 7.32 (d, J=7 Hz, 1H), 7.13 (s, 1H), 7.06 (t, J=8 Hz, 1H), 6.65 (d, J=8 Hz, 1H), 6.28 (d, J=8 Hz, 1H), 3.89 (ABq, Δv1-3=49 Hz, J=17 Hz, 2H), 2.12 (s, 3H); APCI MS m/z=437 (P+1).

Aufarbeitung

  1. temperatureto warm to ambient temperature
  2. stirringstirred 16 hours
  3. customThe reaction was quenched by addition of saturated aqueous bicarbonate
  4. stirringcontinued stirring for 30 minutes
  5. customThe phases were separated
  6. extractionthe aqueous layer was extracted with methylene chloride
  7. washThe combined organic phase was washed with brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated
  10. customThe residue triturated with 50% isopropyl ether/hexane

Quellen und Nachweise

ORD-Eintrag
ord-f73ec43c0cd3492f85130430ded00e5d
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06627755B1

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