반응 #91168

ord-40264fe6f229486c8612a904a343b595

반응 조건

온도
-78°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGstirred at room temperature for 2 hours
  2. 2
    기타After the termination of the reaction
  3. 3
    추출extracted with EtOAc
  4. 4
    기타The organic layer was separated
  5. 5
    건조dried with MgSO4
  6. 6
    농축concentrated under reduced pressure

실험 절차

After 2-chloro-4-hydroxy-benzonitrile (2 g, 0.013 mol) was dissolved in anhydrous THF (40 mL), DIBAL-H 1M hexane solution (21.7 mL, 0.032 mol) was added thereto at −78° C., and the mixture was stirred for 1 hour, and then stirred at room temperature for 2 hours. After the termination of the reaction, the reactant was added with 1M HCl at 0° C. and then extracted with EtOAc. The organic layer was separated, dried with MgSO4, and concentrated under reduced pressure to obtain the title compound, which was used in the next step without a separate purification process.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447044B2uspto-grants-2016_09