Potassium Carbonate → 5-Nitro-2-(2,2,3,3-tetrafluoro-propoxy)pyridine

HRID 450085노트

반응식

HRID 450085 반응식
[F:1][CH:2]([F:8])[C:3]([F:7])([F:6])[CH2:4]I.[N+:9]([C:12]1[CH:13]=[CH:14][C:15]([OH:18])=[N:16][CH:17]=1)([O-:11])=[O:10].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[N+:9]([C:12]1[CH:13]=[CH:14][C:15]([O:18][CH2:4][C:3]([F:7])([F:6])[CH:2]([F:8])[F:1])=[N:16][CH:17]=1)([O-:11])=[O:10]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 5428611,1,2,2-Tetrafluoro-3-iodopropaneHCID 178526703HCID 178526703, 화합물

생성물 1

HCID 866211495-Nitro-2-(2,2,3,3-tetrafluoro-propoxy)pyridine수율 77.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1,1,2,2-Tetrafluoro-3-iodo propane (0.5 g, 2 mmol) was added to a mixture of 5-nitro-2-hydroxy pyridine (860 mg, 6.1 mmol) and potassium carbonate (1.4 g, 10 mmol) in DMF (10 ml) and the reaction heated at reflux for 6 hr. The reaction mixture was cooled to room temperature and filtered. The filtrate was diluted with ethyl acetate (50 ml), washed successively with bicarbonate solution, water, brine, and dried. Concentration to dryness yielded 5-nitro-2-(2,2,3,3-tetrafluoro-propoxy)pyridine (394 mg, 75%) as an oil.

후처리

  1. temperaturethe reaction heated
  2. temperatureat reflux for 6 hr
  3. filtrationfiltered
  4. additionThe filtrate was diluted with ethyl acetate (50 ml)
  5. washwashed successively with bicarbonate solution, water, brine
  6. customdried
  7. concentrationConcentration to dryness

출처 및 근거

ORD 기록
ord-1b8f09e14d914b8a81c0bd7976f8bc58
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486962B2

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