반응 #9515

ord-b29e7842b37f4e659459e8c871f8b783

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The DMF was removed under reduced pressure
  2. 2
    기타the residue was partitioned between dichloromethane (300 mL) and water (150 mL)
  3. 3
    기타The organic layer was separated
  4. 4
    세척washed with brine (120 mL)
  5. 5
    건조dried over magnesium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated

실험 절차

Potassium thioacetate (1.70 g, 14.9 mmol) was added in one portion to a stirred solution of 7-bromo-1-(4-chlorobutyl)-2-ethoxymethyl-1H-imidazo[4,5-c]quinoline (5.37 g, 13.5 mmol) in DMF (65 mL), and the reaction was stirred at ambient temperature for 21 hours. The DMF was removed under reduced pressure, and the residue was partitioned between dichloromethane (300 mL) and water (150 mL). The organic layer was separated, washed with brine (120 mL), dried over magnesium sulfate, filtered, and concentrated to provide 6.09 g of thioacetic acid S-[4-(7-bromo-2-ethoxymethyl-1H-imidazo[4,5-c]quinolin-1-yl)butyl]ester as a brown solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08