반응 #5582

ord-1b45aea4222d4467b64a679104b92b1b

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    workup.STIRRINGthe mixture was stirred under ice-
  3. 3
    온도cooling for 1 hour
  4. 4
    세척The reaction mixture was washed in turn with aqueous saturated sodium bicarbonate and saturated saline
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    workup.DISTILLATIONAfter the solvent was distilled off
  7. 7
    기타the residue was purified by column chromatography (eluent: ethyl acetate)

실험 절차

To 5-(4-amino)butylthioimidazo[1,2-a]pyridine (370 mg, 1.67 mmoles) and triethylamine (0.35 ml, 2.51 mmoles) in methylene chloride (20 ml) was added isopropyl chloroformate (0.25 g, 2.04 mmoles) under ice-cooling with stirring and the mixture was stirred under ice-cooling for 1 hour. The reaction mixture was washed in turn with aqueous saturated sodium bicarbonate and saturated saline, and then dried over anhydrous magnesium sulfate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate) to obtain 215 mg of the desired product (41.8%, light tan oily product).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05244908uspto-grants-1993_09