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2,4,6-Trichloropyrimidine → HCID 19428516, Verbindung

HRID 1721297
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1721297
Cl[C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[NH2:10][CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13]>O1CCCC1>[Cl:9][C:4]1[CH:5]=[C:6]([Cl:8])[N:7]=[C:2]([NH:10][CH2:11][C:12]([CH3:15])([CH3:14])[CH3:13])[N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 773782,4,6-TrichloropyrimidineHCID 79882Neopentylamine

Produkt 1

HCID 19428516HCID 19428516, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

25 g (136.3 mmoles) of 2,4,6-trichloropyrimidine are dropwise added to a mixture of 23.84 g (273.5 mmoles) of 1-amino-2,2-dimethylpropane and 200 ml of tetrahydrofuran at a temperature between 10° C. and 15° C. while stirring and cooling. Thereafter, the reaction mixture is stirred at room temperature for an additional 30 minutes, then evaporated. After distributing the evaporation residue between 300 ml of chloroform and 50 ml of 10% sodium hydroxide solution, the organic phase is separated, washed 4 times with 100 ml of water each, then dried and evaporated. The evaporation residue is subjected to chromatography on a silica gel column. By using a 19:1 mixture of hexane and ethyl acetate, 4,6-dichloro-2-(2,2-dimethylpropylamino)pyrimidine is obtained, which is recrystallized from a mixture of ether and hexane to obtain a yield of 13.60 g (42.6%), m.p.: 63°-66° C.

Aufarbeitung

  1. temperaturecooling
  2. stirringThereafter, the reaction mixture is stirred at room temperature for an additional 30 minutes
  3. customevaporated
  4. customthe organic phase is separated
  5. washwashed 4 times with 100 ml of water each,
  6. customthen dried
  7. customevaporated
  8. additiona 19:1 mixture of hexane and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-f44c43a42904454388914e3ab44a822f
Quelldatensatz
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05510345

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