Hydrogen iodide → 4-(1-(2-(1H-Imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic Acid Salt

HRID 2230619Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2230619
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[N:19]([CH2:20][CH2:21][N:22]3[CH:26]=[CH:25][N:24]=[CH:23]3)[C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=3[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[IH:31]>CO>[IH:31].[N:22]1([CH2:21][CH2:20][N:19]2[C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=3[N:16]=[C:15]2[N:11]2[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]2)[CH:26]=[CH:25][N:24]=[CH:23]1

Komponenten

4

Edukt 2

HCID 24841Hydrogen iodideHCID 184648321-(t-butoxycarbonyl)-4-(1-(2-(1H-imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

Produkt 1

HCID 865838944-(1-(2-(1H-Imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic Acid Salt

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

Combine 1-(t-butoxycarbonyl)-4-(1-(2-(1H-imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (0.22 g, 0.54 mmol), 57% hydriodic acid (0.25 mL, 1.13 mmol), methanol (10 mL) and heat to reflux. After 20 hours, cool the reaction mixture and evaporate in vacuo to give a residue. Triturate the residue with diethyl ether to give a solid. Repeatedly, decant and add diethyl ether before collecting the solid by filtration, rinse with diethyl ether, and dry in vacuo to give the title compound.

Aufarbeitung

  1. temperaturecool the reaction mixture
  2. customevaporate in vacuo
  3. customto give a residue
  4. customTriturate the residue with diethyl ether
  5. customto give a solid
  6. customRepeatedly, decant
  7. additionadd diethyl ether
  8. custombefore collecting the solid
  9. filtrationby filtration
  10. washrinse with diethyl ether
  11. customdry in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f990a1df29be4ed2a8e78fd83f863066
Quelldatensatz
uspto-grants-2002_07
Patentnummer
US06423704B1

Notizen zur Reaktion

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