반응 #76541

ord-fa8383484c864f198b34d46d9af2e65e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도at reflux overnight
  3. 3
    여과filtered
  4. 4
    기타to remove a precipitate
  5. 5
    농축The filtrate was concentrated under vacuum
  6. 6
    세척washed with sodium bicarbonate
  7. 7
    건조with water, and then dried over magnesium sulfate
  8. 8
    여과The solution was filtered through a layer of silica gel eluting first with 1:1 ethyl acetate
  9. 9
    기타The filtrate was evaporated

실험 절차

Propionyl anhydride (20 mL) was added to a suspension of 3-amino-quinoline4-thiol (15 g) in propionic acid (100 mL). The reaction mixture was heated at reflux overnight and then filtered to remove a precipitate. The filtrate was concentrated under vacuum. The residue was taken up in dichloromethane (200 mL), washed with sodium bicarbonate then with water, and then dried over magnesium sulfate. The solution was filtered through a layer of silica gel eluting first with 1:1 ethyl acetate:hexane and then with ethyl acetate. The filtrate was evaporated to provide 2.6 g of 2-ethylthiazolo[4,5-c]quinoline as a yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06703402B2uspto-grants-2004_03