반응 #75000

ord-190279ac6ac94ac49644cabe172141dd

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도chilled (0°) solution
  2. 2
    workup.STIRRINGThe reaction mixture was stirred at ambient temperature for 1 hour
  3. 3
    농축concentrated to dryness under reduced pressure
  4. 4
    workup.ADDITIONThe residue was treated with water
  5. 5
    여과filtered
  6. 6
    기타recrystallized from ethanol

실험 절차

To a stirred and chilled (0°) solution containing 200 g (0.86 mol) of 2-bromo-4-nitrophenylhydrazine (m.p. 143°-145°) and 116.8 g (0.9 mol) of ethyldiisopropylamine in 1000 ml of tetrahydrofuran was added dropwise 108.5 g (0.9 mol) of pivaloyl chloride. The reaction mixture was stirred at ambient temperature for 1 hour and then concentrated to dryness under reduced pressure. The residue was treated with water, filtered and recrystallized from ethanol to give 165 g (52%) of product as a light yellow solid; m.p. 145° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04174958uspto-grants-1979_11