반응 #454409

ord-a011db3510784e24a9dc6d53be72ffe9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the mixture was heated
  2. 2
    온도at reflux for 3 hours
  3. 3
    온도The mixture was cooled
  4. 4
    여과the solids filtered
  5. 5
    세척washed with ethanol
  6. 6
    농축The filtrate was concentrated
  7. 7
    여과collected by filtration
  8. 8
    기타recrystallized from ethanol

실험 절차

To 10.4 g (0.025 mol) of 8-chloro-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2yl-ethyl)-amide in 100 mL of ethanol was added 7.2 g (0.1 mol) of sodium hydrogensulfide and the mixture was heated at reflux for 3 hours. The mixture was cooled and the solids filtered, washed with ethanol, and then with water. The filtrate was concentrated and the solids were suspended in water, collected by filtration, and recrystallized from ethanol to give 6.8 g of the title compound, mp 258-260° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06133270uspto-grants-2000_10