Dimethylformamide → 6-(2-Chloro-2-propenyloxy)-4-methyl-2-n-hexylamino-pyrimidine

HRID 1995026

Reaktionsgleichung

Reaktionsgleichung von HRID 1995026
[OH:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[N:5]=[C:4]([CH3:15])[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[Cl:22][C:23]([CH2:25]Cl)=[CH2:24].CN(C)C=O>O>[Cl:22][C:23](=[CH2:24])[CH2:25][O:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])[N:5]=[C:4]([CH3:15])[CH:3]=1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 65652,3-DichloropropeneHCID 11430Potassium CarbonateHCID 178444746HCID 178444746, Verbindung

Produkt 1

HCID 204887956-(2-Chloro-2-propenyloxy)-4-methyl-2-n-hexylamino-pyrimidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

42.0 g 6-Hydroxy-4-methyl-2-n-hexylamino-pyrimidin (0.2 Mol), 27.6 g K2CO3 (0.2 Mol), 24.4 g 2,3-dichloro-1-propene (0.22 Mol) and 150 ml dimethylformamide are charged in a sulphonation flask. The mixture is heated for about 3 hours at a bath temperature of 110°, then cooled to room temperature and thereafter poured in 500 ml water. This mixture is extracted with ether, the ether extract dried with Na2SO4 and concentrated with the aid of a flask rotary vacuum evaporator at a temperature of up to 60°. The impure title compound is obtained as a brown oil, which is purified chromatographically with ether/hexane 1:3 on silicagel to give a yellow oil that slowly crystallises. m.p. 36°-37°.

Aufarbeitung

  1. temperatureThe mixture is heated for about 3 hours at a bath temperature of 110°
  2. extractionThis mixture is extracted with ether
  3. extractionthe ether extract
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated with the aid of a flask
  6. customrotary vacuum evaporator at a temperature of up to 60°

Quellen und Nachweise

ORD-Eintrag
ord-1d372a172d074845be52f95c6041b800
Quelldatensatz
uspto-grants-1983_09
Patentnummer
US04402730

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