Potassium Iodide → HCID 13319858, Verbindung

HRID 1248485Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1248485
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1[C:9]2[CH:10]=[CH:11][C:12]([F:14])=[CH:13][C:8]=2[O:7][N:6]=1.[CH3:15][CH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O>[ClH:1].[CH3:15][CH:16]1[CH2:21][CH2:20][N:19]([CH2:2][CH2:3][CH2:4][C:5]2[C:9]3[CH:10]=[CH:11][C:12]([F:14])=[CH:13][C:8]=3[O:7][N:6]=2)[CH2:18][CH2:17]1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 693814-MethylpiperidineHCID 109108803-(3-Chloropropyl)-6-fluorobenzo[d]isoxazole

Produkt 1

HCID 13319858HCID 13319858, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 5 g of 3-(3-chloropropyl)-6-fluoro-1,2-benzisoxazole, 2.9 g of 4-methylpiperidine, 10 g of potassium carbonate and a few crystals potassium iodide in 50 ml of dimethylformamide was stirred at 65°-70° C. for four hrs. The mixture was cooled, filtered and concentrated to an oil. The oil was stirred with water and extracted with ether. The organic extracts were washed with water (2×), saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was treated with ethereal hydrogen chloride to give 4 g (55%) or product, mp 180°-182° C. Recrystallization from ethyl acetate/methanol gave the analytical sample, 189°-190° C.

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. filtrationfiltered
  3. concentrationconcentrated to an oil
  4. extractionextracted with ether
  5. washThe organic extracts were washed with water (2×), saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. additionThe residue was treated with ethereal hydrogen chloride
  10. customto give 4 g (55%) or product, mp 180°-182° C
  11. customRecrystallization from ethyl acetate/methanol
  12. customgave the analytical sample, 189°-190° C.

Quellen und Nachweise

ORD-Eintrag
ord-d9979de4e9b340a2a658fee02194e287
Quelldatensatz
uspto-grants-1985_06
Patentnummer
US04524209

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