HCID 15591933, Verbindung → HCID 15591934, Verbindung

HRID 1248369Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1248369
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:9][CH2:10][CH:11]2[CH2:13][C:12]2([Cl:15])[Cl:14])[N:3]=1.[C:16](O)(=[O:18])C.C(OC=O)=O>C(#N)C>[CH:16]([NH:1][C:2]1[N:7]=[C:6]([Cl:8])[CH:5]=[C:4]([NH:9][CH2:10][CH:11]2[CH2:13][C:12]2([Cl:14])[Cl:15])[N:3]=1)=[O:18]

Komponenten

4

Edukt 2

HCID 15591933HCID 15591933, VerbindungHCID 86740153HCID 86740153, Verbindung

Produkt 1

HCID 15591934HCID 15591934, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

A solution of 2.7 g (0.01 mol) of 2-amino-4-chloro-6-{[(2,2-dichloro-cyclopropyl)methyl]amino}pyrimidine in 300 ml of acetonitrile was added dropwise, while stirring, at room temperature over a period of 15 minutes to a solution of 0.9 gm (0.012 mol) of acetic acid-formic acid anhydride in 5 ml of acetonitrile. After stirring the mixture for about 30 hours at room temperature the solvent was distilled off in vacuo, and the residue was treated twice by dissolving it in about 30 ml of toluene and then distilling the toluene off again. The raw product was purified by column chromatography (150 gm silica gel; eluant: Diisopropyl ether/ethyl acetate 9:1), yielding the title compound as white crystals.

Aufarbeitung

  1. distillationwas distilled off in vacuo
  2. additionthe residue was treated twice
  3. dissolutionby dissolving it in about 30 ml of toluene
  4. distillationdistilling the toluene off again
  5. customThe raw product was purified by column chromatography (150 gm silica gel; eluant: Diisopropyl ether/ethyl acetate 9:1)

Quellen und Nachweise

ORD-Eintrag
ord-dfff6a95e9d64e34bc4449bdac0cffe5
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04523945

Notizen zur Reaktion

Wird geladen…