반응 #47199

ord-c84dfea3f23a4a7a83219cb416ea6adc

용매

반응 조건

온도
75°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction was cooled down to room temperature
  2. 2
    추출extracted with ethyl acetate
  3. 3
    기타the crude product was recrystallized from dichloromethane

실험 절차

LiOH monohydrate (0.122 g, 2.90 mmol) was dissolved in 1 mL water and added to methyl 5-tert-butyl-3-nitrothiophene-2-carboxylate (0.235 g, 0.966 mmol) in 3 ml of a 3:1 mixture of THF:MeOH. The resulting mixture was heated at 75° C. for 5 hours. The reaction was cooled down to room temperature, acidified with 1N HCl, extracted with ethyl acetate, and the crude product was recrystallized from dichloromethane:hexane to afford 0.214 g of 5-tert-butyl-3-nitrothiophene-2-carboxylic acid as a yellow solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741479B2uspto-grants-2010_06