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

HRID 450085

反応式

HRID 450085 の反応式
[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]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 5428611,1,2,2-Tetrafluoro-3-iodopropaneHCID 178526703HCID 178526703、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1b8f09e14d914b8a81c0bd7976f8bc58
出典データセット
uspto-grants-2013_07
特許番号
US08486962B2

関連ノート

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