Dichloromethane → HCID 19964159, Verbindung

HRID 977060Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 977060
Cl[S:2]([C:5]1[N:13]=[C:12]2[N:7]([C:8]([O:15][CH3:16])=[N:9][C:10]([CH3:14])=[CH:11]2)[N:6]=1)(=[O:4])=[O:3].[NH2:17][C:18]1[CH:19]=[N:20][CH:21]=[CH:22][C:23]=1[O:24][CH2:25][CH3:26].ClCCl>N1C=CC=CC=1>[CH2:25]([O:24][C:23]1[CH:22]=[CH:21][N:20]=[CH:19][C:18]=1[NH:17][S:2]([C:5]1[N:13]=[C:12]2[N:7]([C:8]([O:15][CH3:16])=[N:9][C:10]([CH3:14])=[CH:11]2)[N:6]=1)(=[O:4])=[O:3])[CH3:26]

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 8172524-ethoxypyridin-3-amineHCID 15003653HCID 15003653, Verbindung

Produkt 1

HCID 19964159HCID 19964159, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

2-Chlorosulfonyl-5-methoxy-7-methyl[1,2,4]triazolo[1,5-c]pyrimidine (1.5 g, 5.7 mmol) was added to a solution of 0.8 g (5.7 mmol) of 3-amino-4-ethoxypyridine in 30 mL of dry pyridine in portions over 10 minutes with stirring. After 16 hours the reaction mixture was poured into 400 mL of dichloromethane. The resulting mixture was washed with 150 mL of water, dried over magnesium smlfate, and filtered. The liltrate was combined with 5 g of silica gel and the mixture was concentrated by evaporation under reduced pressure. The resulting silica plug was placed onto a 200 g silica gel column and eluted with dichloromethane containing increasing amount of ethanol. The product fractions were combined and concentrated by evaporation under reduced pressure and the solid obtained was dried to obtain 0.75 g (36 percent of theory) of the title compound as a white solid melting at 184°-186° C.

Aufarbeitung

  1. washThe resulting mixture was washed with 150 mL of water
  2. dry with materialdried over magnesium smlfate
  3. filtrationfiltered
  4. concentrationthe mixture was concentrated by evaporation under reduced pressure
  5. washeluted with dichloromethane containing
  6. temperatureincreasing amount of ethanol
  7. concentrationconcentrated by evaporation under reduced pressure
  8. customthe solid obtained
  9. customwas dried

Quellen und Nachweise

ORD-Eintrag
ord-e906353c02b447eb8df170b2dffed763
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05614469

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