반응 #11953

ord-b8d808e82a4642758ddd699886c22acc

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while cooling with ice
  2. 2
    기타the solvent was removed by distillation
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in chloroform
  4. 4
    세척washed with 1 mol/l aqueous solution of sodium hydroxide
  5. 5
    건조dried over anhydrous sodium sulfate
  6. 6
    기타The solvent was removed by distillation
  7. 7
    기타The residue was dried under reduced pressure

실험 절차

Commercially available 4-methyl-1-naphthalenecarboxylic acid (250.6 mg) was dissolved in methanol (7.5 ml). Hydrogen chloride gas was blown into the solution for five minutes while cooling with ice. Then, the mixture was stirred for 19 hours at room temperature and the solvent was removed by distillation. The residue was dissolved in chloroform, washed with 1 mol/l aqueous solution of sodium hydroxide, and dried over anhydrous sodium sulfate. The solvent was removed by distillation. The residue was dried under reduced pressure to obtain the target compound (269.9 mg) as colorless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07098215B2uspto-grants-2006_08