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Dimethylformamide → HCID 54753138, Verbindung

HRID 1983847
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1983847
CN(C)C=O.[Br:6][C:7]1[CH:8]=[C:9]([C:13]2[C:22]3[C:17](=[CH:18][C:19]([Cl:24])=[C:20]([CH3:23])[CH:21]=3)[O:16][C:15](=[O:25])[C:14]=2[CH2:26][C:27](O)=[O:28])[CH:10]=[CH:11][CH:12]=1.S(Cl)(Cl)=O.[NH2:34][C:35]1[CH:40]=[CH:39][C:38]([F:41])=[CH:37][C:36]=1[C:42]([F:45])([F:44])[F:43]>O1CCCC1.O.C(#N)C>[Br:6][C:7]1[CH:8]=[C:9]([C:13]2[C:22]3[C:17](=[CH:18][C:19]([Cl:24])=[C:20]([CH3:23])[CH:21]=3)[O:16][C:15](=[O:25])[C:14]=2[CH2:26][C:27]([NH:34][C:35]2[CH:40]=[CH:39][C:38]([F:41])=[CH:37][C:36]=2[C:42]([F:45])([F:43])[F:44])=[O:28])[CH:10]=[CH:11][CH:12]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 6228DimethylformamideHCID 24386Thionyl ChlorideHCID 678534-Fluoro-2-(trifluoromethyl)anilineHCID 54752977HCID 54752977, Verbindung

Produkt 1

HCID 54753138HCID 54753138, VerbindungAusbeute 85,7 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962
Water
Lösungsmittel
HCID 6342AcetonitrileLösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

N,N-Dimethylformamide (0.2 ml) was added to a solution of [4-(3-bromophenyl)-7-chloro-6-methyl-2-oxo-2H-chromen-3-yl]acetic acid (13.5 g) in tetrahydrofuran (135 ml), and then thionyl chloride (5.12 g) was added dropwise to the resulting mixture with passing nitrogen through the reaction vessel at 25° C. After completion of the addition, the mixture was warmed to 40° C. and stirred for 1.5 hours. Then, 2-amino-5-fluorobenzotrifluoride (6.53 g) was added thereto, and the mixture was warmed to 60° C. and then stirred for 2.5 hours. Acetonitrile (67.5 ml) and water (67.5 ml) were added dropwise successively thereto at 40 to 50° C. The resulting mixture was stirred at 40° C. for 1 hour and at 5° C. for 1 hour. Crystals precipitated was collected by filtration, and washed with cold tetrahydrofuran/acetonitrile/water (2/1/1, 40.5 ml). The resulting crystals (17.3 g) were dissolved in acetone (173 ml) by heating. Activated charcoal (0.865 g) was added to the solution, and the mixture was stirred for 10 minutes. The activated charcoal was removed by filtration, and washed with acetone (86.5 ml). The combined filtrate and washings were kept at 40° C., and water (51.9 ml) was added dropwise thereto with stirring. The mixture was cooled to 5° C. and stirred for 1 hour. Crystals were collected by filtration and washed with cold acetone/water (5/1, 51.9 ml) to obtain the title compound (16.1 g, yield 85.7%).

Aufarbeitung

  1. additionAfter completion of the addition
  2. temperaturethe mixture was warmed to 60° C.
  3. stirringstirred for 2.5 hours
  4. customat 40 to 50° C
  5. stirringThe resulting mixture was stirred at 40° C. for 1 hour and at 5° C. for 1 hour
  6. customCrystals precipitated
  7. filtrationwas collected by filtration
  8. washwashed with cold tetrahydrofuran/acetonitrile/water (2/1/1, 40.5 ml)
  9. dissolutionThe resulting crystals (17.3 g) were dissolved in acetone (173 ml)
  10. temperatureby heating
  11. additionActivated charcoal (0.865 g) was added to the solution
  12. stirringthe mixture was stirred for 10 minutes
  13. customThe activated charcoal was removed by filtration
  14. washwashed with acetone (86.5 ml)
  15. customwere kept at 40° C.
  16. additionwater (51.9 ml) was added dropwise
  17. stirringwith stirring
  18. temperatureThe mixture was cooled to 5° C.
  19. stirringstirred for 1 hour
  20. filtrationCrystals were collected by filtration
  21. washwashed with cold acetone/water (5/1, 51.9 ml)

Quellen und Nachweise

ORD-Eintrag
ord-298ff62117f94de895425f65fe3e0c23
Quelldatensatz
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07541478B2

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