Methylhydrazine → 1-methyl-3-pentafluoroethyl-1H-pyrazole

HRID 1843107노트

반응식

HRID 1843107 반응식
[CH3:1][NH:2][NH2:3].C(O/[CH:7]=[CH:8]/[C:9](=O)[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])C>CO>[CH3:1][N:2]1[CH:7]=[CH:8][C:9]([C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])=[N:3]1

참가 물질

4

반응물 2

HCID 6061MethylhydrazineHCID 5906496(1E)-1-ethoxy-4,4,5,5,5-pentafluoropent-1-en-3-one

생성물 1

HCID 229722731-methyl-3-pentafluoroethyl-1H-pyrazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

7.18 g (155.83 mmol) of methylhydrazine are added dropwise to a solution of 30.90 g (141.67 mmol) of (E)-5-ethoxy-1,1,1,2,2-pentafluoropent-4-en-3-one (preparation: Synthesis 2000, 5, 738-42) in 56 ml of methanol and the reaction mixture is heated under reflux for 18 hours. The majority of the methanol is distilled off at atmospheric pressure and the residue is added to ice. The aqueous phase is extracted three times with dichloromethane and the organic phase is then washed three times with saturated sodium chloride solution. After drying over sodium sulphate, the solvent is distilled off at reduced pressure on a rotary evaporator. This gives 15.81 g (52% of theory) of 1-methyl-3-pentafluoroethyl-1H-pyrazole as an oil.

후처리

  1. temperaturethe reaction mixture is heated
  2. temperatureunder reflux for 18 hours
  3. distillationThe majority of the methanol is distilled off at atmospheric pressure
  4. additionthe residue is added to ice
  5. extractionThe aqueous phase is extracted three times with dichloromethane
  6. washthe organic phase is then washed three times with saturated sodium chloride solution
  7. dry with materialAfter drying over sodium sulphate
  8. distillationthe solvent is distilled off at reduced pressure on a rotary evaporator

출처 및 근거

ORD 기록
ord-0083d955867142648b5bfefac529e4db
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946234B2

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