Dichloromethane → HCID 178496341, Verbindung

HRID 2052079Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2052079
[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-56cac8a1c3e9490a9605e7b4eed81a0e
Quelldatensatz
uspto-grants-1980_01
Patentnummer
US04182867

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