Nitric Acid → HCID 178526837、化合物

HRID 573188

反応式

HRID 573188 の反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4]([OH:9])=[N:5][CH:6]=[CH:7][CH:8]=1.S(=O)(=O)(O)O.[N+:17]([O-])([OH:19])=[O:18]>>[N+:17]([C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:10])[F:11])[C:4]([OH:9])=[N:5][CH:6]=1)([O-:19])=[O:18]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 36784112(1H)-Pyridinone, 3-(trifluoromethyl)-

生成物 1

HCID 178526837HCID 178526837、化合物

反応条件

温度
0 °C

実験手順

3-(Trifluoromethyl)pyridin-2-ol (2.3 g) was added to concentrated sulfuric acid (15 mL) at 0° C. The mixture was stirred at 0° C. for 5 minutes. To this solution was added nitric acid (fuming, 6 mL) dropwise over 5 minutes. The reaction mixture was stirred at room temperature for 2 hours, and then heated at 50° C. for 3 hours. After cooling, the reaction mixture was poured into ice (200 g), and the mixture was extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried over MgSO4, filtered, and concentrated under reduced pressure to give the title compound.

後処理

  1. stirringThe reaction mixture was stirred at room temperature for 2 hours
  2. temperatureheated at 50° C. for 3 hours
  3. temperatureAfter cooling
  4. extractionthe mixture was extracted with ethyl acetate three times
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-86570945c10448b6b884dda0ab05615e
出典データセット
uspto-grants-2015_05
特許番号
US09029404B2

関連ノート

読み込み中…