Potassium Carbonate → HCID 15020605, Verbindung

HRID 1493171

Reaktionsgleichung

Reaktionsgleichung von HRID 1493171
[CH:1]12[CH2:8][CH:5]([CH2:6][CH2:7]1)[CH2:4][CH2:3][C:2]2=O.[F:10][C:11]1[CH:21]=[CH:20][C:14]([C:15]([CH2:17][C:18]#[N:19])=O)=[CH:13][CH:12]=1.C(=O)([O-])[O-:23].[K+].[K+]>ClC(Cl)C(Cl)Cl>[F:10][C:11]1[CH:21]=[CH:20][C:14]([C:15]2[C:3]3[CH2:4][CH:5]4[CH2:8][CH:1]([CH2:7][CH2:6]4)[C:2]=3[NH:19][C:18](=[O:23])[CH:17]=2)=[CH:13][CH:12]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 107363Bicyclo[3.2.1]octan-2-oneHCID 2783172p-Fluorobenzoylacetonitrile

Produkt 1

HCID 15020605HCID 15020605, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 65911,1,2,2-TetrachloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

Bicyclo[3.2.1]octan-2-one (2 g) and 4-fluorobenzoylacetonitrile (2.6 g) are dissolved in 1,1,2,2-tetrachloroethane (5 ml) and thereto is added 75% polyphosphoric acid (25 g). The mixture is stirred at 80° C. for 30 minutes, at 100° C. for 1 hour, and further at 130° C. for 30 minutes. After cooling, the reaction mixture is poured into ice-water and neutralized with potassium carbonate. The precipitated crystals are collected by filtration and washed successively with water and ethyl acetate. The resultant is recrystallized from methanol to give the desired product (2.7 g), m.p.>300° C.

Aufarbeitung

  1. waitfurther at 130° C. for 30 minutes
  2. temperatureAfter cooling
  3. filtrationThe precipitated crystals are collected by filtration
  4. washwashed successively with water and ethyl acetate
  5. customThe resultant is recrystallized from methanol

Quellen und Nachweise

ORD-Eintrag
ord-d3a5ee99b987431495d38437d6e93bc1
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05021421

Verknüpfte Notizen

Wird geladen…