Dichloromethane → HCID 178496341, Verbindung

HRID 46838

Reaktionsgleichung

Reaktionsgleichung von HRID 46838
[NH2:1][C:2]1[N+:7]([O-:8])=[C:6]([NH2:9])[CH:5]=[C:4]([N:10]2[CH2:15][CH:14]=[CH:13][CH2:12][CH2:11]2)[N:3]=1.C(Cl)Cl.[CH3:19][O:20][CH2:21][CH2:22][O:23][C:24](Cl)=[O:25]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:22][CH2:21][O:20][CH3:19])=[O:25])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 694002-Methoxyethyl chloroformateHCID 178507852HCID 178507852, Verbindung

Produkt 1

HCID 178496341HCID 178496341, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

10 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are stirred at 5° C. in 150 ml. of methylene chloride and 30 ml. of triethylamine and treated with 20 ml. of chloroformic acid 2-methoxyethyl ester. The mixture is stirred at room temperature for 4 hours, then washed with water and extracted with methylene chloride. The organic phases are evaporated under reduced pressure and the residue is recrystallized from diethyl ether, there being obtained bis(2-methoxyethyl) 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 126°-128° C.

Aufarbeitung

  1. washwashed with water
  2. extractionextracted with methylene chloride
  3. customThe organic phases are evaporated under reduced pressure
  4. customthe residue is recrystallized from diethyl ether, there

Quellen und Nachweise

ORD-Eintrag
ord-8a990e8610d14b2e90e8631959b728bb
Quelldatensatz
uspto-grants-1979_11
Patentnummer
US04175189

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