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Dimethylamine → 2-Dimethylamino-4-sec. butylamino-5-nitro-6-methylpyrimidine

HRID 597468
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 597468
Cl[C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH2:11][CH3:12])[CH3:10])[C:5]([N+:13]([O-:15])=[O:14])=[C:4]([CH3:16])[N:3]=1.[CH3:17][NH:18][CH3:19]>C(N(CC)CC)C>[CH3:17][N:18]([CH3:19])[C:2]1[N:7]=[C:6]([NH:8][CH:9]([CH2:11][CH3:12])[CH3:10])[C:5]([N+:13]([O-:15])=[O:14])=[C:4]([CH3:16])[N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 674DimethylamineHCID 188014492-Chloro-4-sec. butylamino-5-nitro-6-methylpyrimidine

Produkt 1

HCID 1317106992-Dimethylamino-4-sec. butylamino-5-nitro-6-methylpyrimidineAusbeute 98,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

10 ml of triethylamine are added to a solution of 15.9 g of 2-chloro-4-sec. butylamino-5-nitro-6-methylpyrimidine (0.065 mole) in 250 ml of alcohol. Then 4.5 g (0.1 mole) of dimethylamine are passed in and the mixture is boiled for 4 hours at 100° C. After it has cooled, the mixture is evaporated and the residue is suspended in water. The resultant precipitate is filtered off with suction and washed with water until no more chlorine ions are dissolved out. The product is dried in a water jet vacuum at 50° C to yield 16.2 g of 2-dimethylamino-4-sec. butylamino-5-nitro-6-methylpyrimidine (=98.5% yield) of m.p. 98°-100° C. On recrystallisation from petroleum ether, the melting point of the product rises to 109°-110° C.

Aufarbeitung

  1. temperatureAfter it has cooled
  2. customthe mixture is evaporated
  3. filtrationThe resultant precipitate is filtered off with suction
  4. washwashed with water until no more chlorine ions
  5. dissolutionare dissolved out
  6. dry with materialThe product is dried in a water jet vacuum at 50° C

Quellen und Nachweise

ORD-Eintrag
ord-ee187218e1834252a4c18fd108ecbe5e
Quelldatensatz
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04014677

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