Ethanol → HCID 178474266, Verbindung

HRID 493387

Reaktionsgleichung

Reaktionsgleichung von HRID 493387
[O:1]([CH2:8][C:9]1[NH:10][CH:11]=[C:12]([C:14]2[CH:27]=[CH:26][C:17]([O:18][C:19]3[CH:25]=[CH:24][C:22]([NH2:23])=[CH:21][CH:20]=3)=[CH:16][CH:15]=2)[N:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.CI.[CH2:37]([OH:39])[CH3:38]>>[O:1]([CH2:8][C:9]1[NH:10][CH:11]=[C:12]([C:14]2[CH:27]=[CH:26][C:17]([O:18][C:19]3[CH:20]=[CH:21][C:22]([NH:23][C:37](=[O:39])[CH3:38])=[CH:24][CH:25]=3)=[CH:16][CH:15]=2)[N:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 4

HCID 702EthanolHCID 6328Methyl iodideHCID 8471TriethylamineHCID 178507748HCID 178507748, Verbindung

Produkt 1

HCID 178474266HCID 178474266, Verbindung

Versuchsvorschrift

4-{4-[2-(phenoxymethyl)-1H-imidazol-4-yl]phenoxy}aniline (600 mg, 0.00168 mol), (prepared according to a method analogous to that described in Example 28) is suspended in ethanol (30 ml) at 0° C. Triethylamine (0.235 ml, 0.00168 mol) and methyl iodide (0.136 ml, 0.0022 mol) are added. The mixture is stirred for 20 hours then evaporated to dryness. The residue obtained is adsorbed on silica then purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 4-6 to 5-5). After washing with diethyl ether and isopentane, a beige-coloured powder is obtained.

Aufarbeitung

  1. customthen evaporated to dryness
  2. customThe residue obtained
  3. customthen purified by chromatography on a Biotage-type silica column (eluent: ethyl acetate-heptane: 4-6 to 5-5)
  4. washAfter washing with diethyl ether and isopentane
  5. customa beige-coloured powder is obtained

Quellen und Nachweise

ORD-Eintrag
ord-b665d5e41fa942deb301be4134808e4c
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07534805B2

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