Water → 6-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine

HRID 2389734

Reaktionsgleichung

Reaktionsgleichung von HRID 2389734
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][C:9]=2[Cl:15])[NH:5][C:4](=[S:16])[N:3]=1.I[CH2:18][CH3:19].C(=O)(O)[O-].[Na+].O>CS(C)=O>[Cl:15][C:9]1[CH:10]=[C:11]([Cl:14])[CH:12]=[CH:13][C:8]=1[C:6]1[N:5]=[C:4]([S:16][CH2:18][CH3:19])[N:3]=[C:2]([NH2:1])[CH:7]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6340IodoethaneHCID 516892Sodium BicarbonateHCID 583059934-Amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione

Produkt 1

HCID 583060056-(2,4-Dichlorophenyl)-2-(ethylthio)pyrimidine-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

67.5 g (248 mmol) of 4-amino-6-(2,4-dichlorophenyl)pyrimidine-2(1H)-thione and 77.37 g (496.04 mmol) of iodoethane are dissolved in 560 ml of dry DMSO and, at RT, 270 ml of a saturated aqueous sodium bicarbonate solution are slowly added. The mixture is stirred at RT for 5 h and then 440 ml of water are added. The precipitate is filtered off with suction, washed with water and sucked dry. It is stirred twice with 100 ml of isopropanol each time and again filtered off with suction. It is washed once more with petroleum ether and the residue is dried under high vacuum. 50.0 g (67% of theory) of the product are obtained as a solid.

Aufarbeitung

  1. filtrationThe precipitate is filtered off with suction
  2. washwashed with water
  3. customsucked dry
  4. stirringIt is stirred twice with 100 ml of isopropanol each time
  5. filtrationagain filtered off with suction
  6. washIt is washed once more with petroleum ether
  7. customthe residue is dried under high vacuum
  8. custom50.0 g (67% of theory) of the product are obtained as a solid

Quellen und Nachweise

ORD-Eintrag
ord-b36d2978298b4e7a9f7c9425e1fc4cc1
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08273752B2

Verknüpfte Notizen

Wird geladen…