Potassium Iodide → HCID 90182633, Verbindung

HRID 1482619Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1482619
Cl[CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]=[N:6]1.[NH:14]1[CH2:19][CH2:18][CH:17]([C:20]2[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=3[O:22][N:21]=2)[CH2:16][CH2:15]1.C(N(C(C)C)CC)(C)C.[I-].[K+]>C(#N)C>[N:5]1([CH2:4][CH2:3][CH2:2][N:14]2[CH2:15][CH2:16][CH:17]([C:20]3[C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][C:23]=4[O:22][N:21]=3)[CH2:18][CH2:19]2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[N:7]=[N:6]1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 52439381-(3-chloropropyl)-1H-1,2,3-benzotriazoleHCID 130764363-(Piperidin-4-yl)benzo[d]isoxazole

Produkt 1

HCID 90182633HCID 90182633, VerbindungAusbeute 69,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1-(3-chloropropyl)-1H-benzotriazole (11.7 g, 0.06 mol) was dissolved into 150 ml of acetonitrile, 3-(piperidine-4-yl)benzisoxazole (10.1 g, 0.05 mol), diisopropylethylamine (25.8 g, 0.02 mol) and potassium iodide (8.3 g, 0.05 mol) were respectively added. The mixture was stirred and mixed, then heated and refluxed to react for 15 hours. The mixture was cooled down to ambient temperature and filtered. The filtrate was concentrated to produce oily products, and treated by chromatography with neutral Al2O3 and purified, eluted with dichloromethane to produce 12.6 g compound (I-84) with a yield of 69.7%. ESI-MS [M+H]+: m/z 362.2.

Aufarbeitung

  1. additionwere respectively added
  2. additionmixed
  3. temperatureheated
  4. temperaturerefluxed
  5. customto react for 15 hours
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. customto produce oily products
  9. additiontreated by chromatography with neutral Al2O3
  10. custompurified
  11. washeluted with dichloromethane

Quellen und Nachweise

ORD-Eintrag
ord-5fcd02acdc344021bb90a0699580be7e
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09415047B2

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