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Hydrochloric Acid → 6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H)-quinolinone

HRID 1904660
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1904660
C(NC(C)C)(C)C.C([Li])CCC.CC(C)=O.[C:17](=[O:19])=O.[Cl:20][C:21]1[CH:22]=[C:23]2[C:28](=[CH:29][CH:30]=1)[N:27]([C:31](=[O:40])[C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:33]=1[Cl:39])[CH2:26][CH2:25][C:24]2=O.CI.Cl>O1CCCC1.C(OCC)(=O)C.O.CCCCCC>[Cl:20][C:21]1[CH:30]=[C:29]2[C:28](=[CH:23][CH:22]=1)[N:27]([C:31](=[O:40])[C:32]1[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][C:33]=1[Cl:39])[CH2:26][CH:25]([CH3:24])[C:17]2=[O:19]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

11

Edukt 6

HCID 313Hydrochloric AcidHCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 10522118HCID 10522118, VerbindungHCID 18522661Acetone cardiceHCID 178418339Butyllithium

Produkt 1

HCID 14501493
6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H)-quinolinone

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×HCID 8058HexaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a cooled (-20° C. to -15° C.) solution of diisopropylamine (4.7 g) in anhydrous tetrahydrofuran (100 ml) was added dropwise n-hexane solution (29 ml) of 1.6 N butyl lithium over a 30-minute period in a nitrogen atmosphere, and stirring was continued for 30 minutes after the mixed solution was returned to 0° C. Then the solution was cooled to -75° C. with acetone-dry ice and 15 g of 6-chloro-1-(2,4dichloro-benzoyl)-2,3-dihydro-4(1H)-quinolinone dissolved in 150 ml of anhydrous tetrahydrofuran was added dropwise over a 1-hour period. The reaction mixture was stirred for another 1 hour at -75° C., and methyl iodide (18 g) was added dropwise with stirring over a 30-minute period. The reaction mixture was then slowly warmed to 0° C. over two hour, and acidified under cooling with 2 N hydrochloric acid to be weakly acidic. The reaction mixture was poured into 300 ml of water, then shaken with ethyl acetate (500 ml). The organic layer was washed once with saturated aqueous NaCl solution (200 ml) and dried over anhydrous sodium aulfate. Ethyl acetate was removed in vacuo and the residue was subjected to silica gel column chromatography using a hexane-ethyl acetate mixture (4: 1) to obtain 6-chloro-1-(2,4-dichlorobenzoyl)-2,3-dihydro-3-methyl-4(1H) -quinolinone (yield 7.8 g) as white crystal.

Aufarbeitung

  1. customwas returned to 0° C
  2. additionwas added dropwise over a 1-hour period
  3. stirringThe reaction mixture was stirred for another 1 hour at -75° C.
  4. stirringwith stirring over a 30-minute period
  5. washThe organic layer was washed once with saturated aqueous NaCl solution (200 ml)
  6. dry with materialdried over anhydrous sodium aulfate
  7. customEthyl acetate was removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-fb69d89175444380962b69ada026a12a
Quelldatensatz
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04839368

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