Dichloromethane → HCID 178452819, Verbindung

HRID 26443

Reaktionsgleichung

Reaktionsgleichung von HRID 26443
[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.[CH2:19]([O:23][C:24](Cl)=[O:25])[CH2:20][CH2:21][CH3:22]>C(N(CC)CC)C>[N:10]1([C:4]2[N:3]=[C:2]([NH:1][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[O:25])[N+:7]([O-:8])=[C:6]([NH:9][C:24]([O:23][CH2:19][CH2:20][CH2:21][CH3:22])=[O:25])[CH:5]=2)[CH2:11][CH:12]=[CH:13][CH2:14][CH2:15]1

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 61140Butyl chloroformateHCID 178507852HCID 178507852, Verbindung

Produkt 1

HCID 178452819HCID 178452819, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

20 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed with 250 ml. of methylene chloride and 35 ml. of triethylamine, stirred and cooled to 5° C. The mixture is treated with 45 ml. of chloroformic acid butyl ester and stirred at room temperature for 6 hours. The mixture obtained is washed with water, extracted with methylene chloride and evaporated under reduced pressure. The residue is recrystallized from ethanol, there being obtained dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 131°-132° C.

Aufarbeitung

  1. additionThe mixture is treated with 45 ml
  2. customThe mixture obtained
  3. washis washed with water
  4. extractionextracted with methylene chloride
  5. customevaporated under reduced pressure
  6. customThe residue is recrystallized from ethanol, there

Quellen und Nachweise

ORD-Eintrag
ord-aaf95424dd714d558075c4f775f387bd
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150132

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