Hydrochloric Acid → 2-Chloro-4-(2,5-dichloroanilino)pyrimidine

HRID 347742

Reaktionsgleichung

Reaktionsgleichung von HRID 347742
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[Cl:9][C:10]1[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][C:11]=1[NH2:12].Cl>C(O)CCC>[Cl:1][C:2]1[N:7]=[C:6]([NH:12][C:11]2[CH:13]=[C:14]([Cl:17])[CH:15]=[CH:16][C:10]=2[Cl:9])[CH:5]=[CH:4][N:3]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 72622,5-DichloroanilineHCID 775312,4-Dichloropyrimidine

Produkt 1

HCID 179811312-Chloro-4-(2,5-dichloroanilino)pyrimidineAusbeute 20 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Versuchsvorschrift

2,4-Dichloropyrimidine (50 g, 0.34 mol), 2,5-dichloroaniline (54.38 g, 0.34 mol) and concentrated hydrochloric acid (cat. amount) were dissolved in n-butanol (250 ml). The reaction mixture was stirred at room temperature for 12 hours after which the solid that had formed was collected by filtration. The organics were allowed to stand for 48 hours and the solid that formed was collected by filtration, washed with EtOAc and dried to give the title product as a white solid (18.65 g). NMR (300 MHz): 6.82 (d, 1H), 7.31 (dd, 1H), 7.58 (d, 1H), 7.82 (s, 1H), 8.19 (d, 1H), 9.82 (s, 1H); m/z: (ES+) 273.9 (MH+).

Aufarbeitung

  1. customthat had formed
  2. filtrationwas collected by filtration
  3. waitto stand for 48 hours
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. washwashed with EtOAc
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-44c263d9e5d5409fb10eec7b770bee1f
Quelldatensatz
uspto-grants-2007_02
Patentnummer
US07176212B2

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