1,2-Dichloroethane → HCID 13980725, Verbindung

HRID 461309Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 461309
C([C:7]1[CH:12]=[CH:11][N:10]=[C:9]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=O)=[CH:15][CH:14]=2)[N:8]=1)CCCCC.[CH2:22](Cl)[CH2:23]Cl.P(Cl)(Cl)(Cl)=O>CCOCC>[CH2:9]([C:12]1[CH:11]=[N:10][C:9]([C:13]2[CH:14]=[CH:15][C:16]([C:17]#[N:19])=[CH:20][CH:21]=2)=[N:8][CH:7]=1)[CH2:13][CH2:14][CH2:15][CH2:22][CH3:23]

Komponenten

5

Edukt 3

HCID 111,2-DichloroethaneHCID 24813Phosphorus oxychlorideHCID 541836714-(4-n-Hexylpyrimid-2-yl)benzoic acid amide

Produkt 1

HCID 13980725HCID 13980725, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

15.58 g. of 4-(4-n-hexylpyrimid-2-yl)benzoic acid amide are left in a mixture of 350 ml. of ethylene chloride and 5.58 ml. of phosphorus oxychloride for 90 minutes under reflux, with stirring. The reaction mixture, diluted with ether, is washed with 2N sodium hydroxide solution and then with water until neutral. After evaporation of the organic phase, drying over sodium sulfate, 14.6 g. of 5-n-hexyl-2-(4-cyanophenyl)pyrimidine result, which are distilled in high vacuum, m.p. 53.5° - 54.5°; cl.p. 35.5° - 36.5°.

Aufarbeitung

  1. washis washed with 2N sodium hydroxide solution
  2. customAfter evaporation of the organic phase
  3. dry with materialdrying over sodium sulfate, 14.6 g

Quellen und Nachweise

ORD-Eintrag
ord-37d61fc84d3a426d9c6824b870649a10
Quelldatensatz
uspto-grants-1977_12
Patentnummer
US04062798

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