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Sulfuric Acid → 3,4-Dihydro-3-[(3-pyridinylmethyl)amino]-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone

HRID 1663295
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1663295
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH:7]=[N:8][N:9]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:19]([F:28])([C:24]([F:27])([F:26])[F:25])[C:20]([F:23])([F:22])[F:21])[CH:16]=3)[NH:11][C:10]2=[O:29])[CH:2]=1.S(=O)(=O)(O)O>[C].[Pd].[I-].[K+].CN(C)C=O>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][NH:8][N:9]2[CH2:18][C:17]3[C:12](=[CH:13][CH:14]=[C:15]([C:19]([F:28])([C:24]([F:25])([F:26])[F:27])[C:20]([F:21])([F:23])[F:22])[CH:16]=3)[NH:11][C:10]2=[O:29])[CH:2]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 1118Sulfuric AcidHCID 730165883,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone

Produkt 1

HCID 231109103,4-Dihydro-3-[(3-pyridinylmethyl)amino]-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinoneAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 4875Potassium IodideKatalysator
HCID 178418390
HCID 178418390, Verbindung
Katalysator
HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

In a 200-ml autoclave were placed 8.40 g (20 mmol) of 3,4-dihydro-3-(3-pyridylmethylideneamino)-6-[1,2,2,2-tetrafluoro-1-(trifluoromethyl)ethyl]-2(1H)-quinazolinone, 0.21 g (0.05 mmol) of 5% palladium-carbon (containing 50% water), 1.68 mg (0.01 mmol) of potassium iodide, 0.4 g (98%, 4 mmol) of concentrated sulfuric acid and 50 ml of dimethylformamide. They were heated to 45° C. with stirring and the reaction was carried out at a hydrogen pressure of 2 kg/cm2 until the hydrogen absorption rate decreased. After the reaction mixture was cooled to room temperature, the catalyst was removed by filtration. The filtrate was poured into 100 ml of water and the crystals precipitated were collected by filtration. The crystals were recrystallized from toluene to obtain 8.02 g of the desired compound.

Aufarbeitung

  1. customthe reaction was carried out at a hydrogen pressure of 2 kg/cm2 until the hydrogen absorption rate
  2. temperatureAfter the reaction mixture was cooled to room temperature
  3. customthe catalyst was removed by filtration
  4. additionThe filtrate was poured into 100 ml of water
  5. customthe crystals precipitated
  6. filtrationwere collected by filtration
  7. customThe crystals were recrystallized from toluene

Quellen und Nachweise

ORD-Eintrag
ord-f2aa66f9773647bda0d56847f9db023a
Quelldatensatz
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08034931B2

Notizen zur Reaktion

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