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Ethylamine → 4-Chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

HRID 372642
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 372642
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:10])[N:5]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:3]=1.[CH2:15]([NH2:17])[CH3:16]>CC(C)=O>[Cl:10][C:6]1[C:7]([C:8]#[N:9])=[C:2]([NH:17][CH2:15][CH3:16])[N:3]=[C:4]([NH:11][CH:12]([CH3:14])[CH3:13])[N:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 6341EthylamineHCID 205102654,6-Dichloro-2-isopropylamino-5-pyrimidinecarbonitrile

Produkt 1

HCID 205102154-Chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Versuchsvorschrift

A stirred solution of 3.5 grams of 4,6-dichloro-2-isopropylamino-5-pyrimidinecarbonitrile in 100 ml of acetone was cooled to between 0° and -5°; a solution of 2.1 grams of aqueous 70% ethylamine in 25 ml of acetone was added dropwise. Upon complete addition, the reaction mixture was warmed to room temperature and stirred for 18 hours. The acetone was removed under reduced pressure, and the residue was extracted with a mixture of diethyl ether and water. The organic layer was separated and dried over magnesium sulfate. The mixture was filtered, and the filtrate was evaporated to dryness under reduced pressure. The residue was recrystallized from methylcyclohexane to give 3.1 grams of 4-chloro-6-ethylamino-2-isopropylamino-5-pyrimidinecarbonitrile; mp, 144°-146°.

Aufarbeitung

  1. additionUpon complete addition
  2. customThe acetone was removed under reduced pressure
  3. extractionthe residue was extracted with a mixture of diethyl ether and water
  4. customThe organic layer was separated
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe mixture was filtered
  7. customthe filtrate was evaporated to dryness under reduced pressure
  8. customThe residue was recrystallized from methylcyclohexane

Quellen und Nachweise

ORD-Eintrag
ord-56808d51d50e4ea6b902d37b407e4b43
Quelldatensatz
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04092150

Notizen zur Reaktion

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