Sodium Iodide → HCID 67599459, Verbindung

HRID 582547

Reaktionsgleichung

Reaktionsgleichung von HRID 582547
[Br:1][C:2]1[C:3]([NH:10][CH2:11][CH:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:16]=2[CH3:22])[CH3:13])=[N:4][CH:5]=[N:6][C:7]=1[CH2:8][CH3:9].[C:23]([O:31][CH2:32]Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[I-:34].[Na+]>CC(C)=O>[I-:34].[C:23]([O:31][CH2:32][N+:6]1[C:7]([CH2:8][CH3:9])=[C:2]([Br:1])[C:3]([NH:10][CH2:11][CH:12]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][C:16]=2[CH3:22])[CH3:13])=[N:4][CH:5]=1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Komponenten

5

Edukt 3

HCID 5238Sodium IodideHCID 79257Chloromethyl benzoateHCID 537398875-Bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine

Produkt 1

HCID 67599459HCID 67599459, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

0.3 g (8.2 mmol) of 5-bromo-6-ethyl-4-[2-(2,4-dimethylphenoxy)-propylamino]pyrimidine (according to EP-A-57 440), 0.17 g (9.8 mmol) of chloromethyl benzoate and 0.12 g (8.2 mmol) of sodium iodide in 25 ml of acetone were heated under reflux for 8 hours. After cooling, the precipitated sodium chloride was filtered off and the filtrate was concentrated. The residue was taken up in dichloromethane and washed by stirring with water. The organic phase was dried and concentrated. The residue was digested with ethyl acetate. Filtration with suction gave 0.97 g (53.3% of theory) of light-yellow crystals. mp.: 159-161° C.

Aufarbeitung

  1. temperatureunder reflux for 8 hours
  2. temperatureAfter cooling
  3. filtrationthe precipitated sodium chloride was filtered off
  4. concentrationthe filtrate was concentrated
  5. washwashed
  6. customThe organic phase was dried
  7. concentrationconcentrated
  8. filtrationFiltration with suction
  9. customgave 0.97 g (53.3% of theory) of light-yellow crystals

Quellen und Nachweise

ORD-Eintrag
ord-f8a076c500ce4ebcb8ed728ba249b303
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05925644

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