Potassium Iodide → HCID 118386857, Verbindung

HRID 1482597Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1482597
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.[CH3:14][C:15]1[CH:16]=[C:17]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH:18]=[CH:19][CH:20]=1.[CH:27](N(C(C)C)CC)(C)C.[I-].[K+]>C(#N)C>[CH3:14][C:15]1[CH:16]=[C:17]([N:21]2[CH2:26][CH2:25][N:24]([CH:2]([CH3:27])[CH2:3][CH2:4][N:5]3[C:9]4[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=4[N:7]=[N:6]3)[CH2:23][CH2:22]2)[CH:18]=[CH:19][CH:20]=1

Komponenten

6

Edukt 4

HCID 4875Potassium IodideHCID 81531DiisopropylethylamineHCID 831111-(m-Tolyl)piperazineHCID 52439381-(3-chloropropyl)-1H-1,2,3-benzotriazole

Produkt 1

HCID 118386857HCID 118386857, VerbindungAusbeute 74,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

1-(3-chloropropyl)-1H-benzotriazole (7.02 g, 0.036 mol) was dissolved into 100 ml of acetonitrile, 3-methyl phenylpiperazine (5.3 g, 0.03 mol), diisopropylethylamine (15.5 g, 0.12 mol) and potassium iodide (5.0 g, 0.03 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 7.5 g compound (I-39) with a yield of 74.6%. ESI-MS [M+H]+: m/z 335.2.

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-80899602045c40f2b6cffc09c72f72d8
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09415047B2

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