Hydrochloric Acid → HCID 178440798, Verbindung

HRID 1279497Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1279497
C1(C(C2C=CC=CC=2)(C2C=CC=CC=2)[N:8]2[CH:12]=[C:11]([CH2:13][CH2:14][C:15]#[C:16][CH2:17][CH2:18][CH:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[N:10]=[CH:9]2)C=CC=CC=1.Cl>C(O)C>[NH:8]1[CH:12]=[C:11]([CH2:13][CH2:14][C:15]#[C:16][CH2:17][CH2:18][CH:19]2[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24]2)[N:10]=[CH:9]1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 184283751-[1-triphenylmethyl-1H-imidazol-4-yl]-6-cyclohexyl-3-hexyne

Produkt 1

HCID 178440798HCID 178440798, VerbindungAusbeute 105,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

1-[1-Triphenylmethyl-1H-imidazol-4-yl]-6-cyclohexyl-3-hexyne (0.30 gram, 0.64 mmol) was dissolved in ethanol (10 ml). 2N HCl (20 ml) was added, and the mixture heated at 90° C. for 1 hour. The reaction mixture was cooled, filtered, and the filtrate neutralized with 10% NaOH solution and then partitioned between chloroform and water. The chloroform layer was separated, dried over Na2SO4, filtered and evaporated in vacuo to obtain the crude oil. The crude product was purified using column chromatography using MeOH/CHCl3, 10:90 to afford 155 mgs of 1-[1H-imidazol-4-yl]-6-cyclohexyl-3-hexyne (23).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. filtrationfiltered
  3. custompartitioned between chloroform and water
  4. customThe chloroform layer was separated
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customto obtain the crude oil
  9. customThe crude product was purified

Quellen und Nachweise

ORD-Eintrag
ord-b150a7e1866447ef9222bd3eb5791c0f
Quelldatensatz
uspto-grants-2002_09
Patentnummer
US06448282B1

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