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Diisopropylethylamine → 2-[3-(4-cyanobenzyl)-3H-imidazol-1-yl]-N-(4-cyanobenzyl)-N-(1-phenylpiperidin-4-yl)acetamide hydrochloride

HRID 1068505
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1068505
[C:1]([C:3]1[CH:22]=[CH:21][C:6]([CH2:7][NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1)#[N:2].[C:23]([C:25]1[CH:40]=[CH:39][C:28]([CH2:29][N:30]2[C:34](CC([O-])=O)=[CH:33][N:32]=[CH:31]2)=[CH:27][CH:26]=1)#[N:24].[Li+].[OH2:42].ON1C2C=CC=[CH:52][C:47]=2N=N1.[ClH:53].CN(C)CCCN=C=NCC.C(N(CC)C(C)C)(C)C>>[ClH:53].[C:23]([C:25]1[CH:26]=[CH:27][C:28]([CH2:29][N:30]2[CH:34]=[CH:33][N:32]([CH2:47][C:52]([N:8]([CH2:7][C:6]3[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:22][CH:21]=3)[CH:9]3[CH2:10][CH2:11][N:12]([C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH2:13][CH2:14]3)=[O:42])[CH2:31]2)=[CH:39][CH:40]=1)#[N:24]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 21193414HCID 21193414, VerbindungHCID 67586058HCID 67586058, Verbindung

Produkt 1

HCID 21193223
2-[3-(4-cyanobenzyl)-3H-imidazol-1-yl]-N-(4-cyanobenzyl)-N-(1-phenylpiperidin-4-yl)acetamide hydrochloride

Versuchsvorschrift

4-Cyanobenzyl(1-phenylpiperidin-4-yl)amine (75 mg, 0.26 mmol), lithium [3-(4-cyanobenzyl)-3H-imidazol-4-yl]acetate (70 mg, 0.28 mmol), 1-hydroxybenzotriazole hydrate (52 mg, 0.38 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (99 mg, 0.52 mmol), and N,N-diisopropylethylamine (67 μL, 0.38 mmol) were added to degassed DMF (3 mL) and the mixture was stirred for 18 hrs at room temperature then concentrated in vacuo. The residue was added to sat. NaHCO3(aq) (5 mL) and extracted with dichloromethane (3×3 mL). The combined organic extracts were dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was chromatographed on silica gel, eluting with dichloromethane—2% methanol to give the product as a free base. This was lyophilized from HCl (aq)—acetonitrile to give the title compound as a white solid.

Aufarbeitung

  1. customto degassed DMF (3 mL)
  2. concentrationthen concentrated in vacuo
  3. additionThe residue was added to sat. NaHCO3(aq) (5 mL)
  4. extractionextracted with dichloromethane (3×3 mL)
  5. dry with materialThe combined organic extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was chromatographed on silica gel
  9. washeluting with dichloromethane—2% methanol
  10. customto give the product as a free base

Quellen und Nachweise

ORD-Eintrag
ord-836791aa023346fe8a3c580e4633ac28
Quelldatensatz
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06248756B1

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