Dimethyl Sulfoxide → Ethyl 2-(3-(trifluoromethyl)pyridin-2-yl)acetate

HRID 1907678

反応式

HRID 1907678 の反応式
[F:1][C:2]([F:21])([F:20])[C:3]1[C:4]([CH:9](C(OCC)=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:5][CH:6]=[CH:7][CH:8]=1.CS(C)=O.[Cl-].[Na+]>O>[F:21][C:2]([F:1])([F:20])[C:3]1[C:4]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:5][CH:6]=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 57950213Diethyl 2-(3-(trifluoromethyl)pyridin-2-yl)malonate

生成物 1

HCID 57447456Ethyl 2-(3-(trifluoromethyl)pyridin-2-yl)acetate収率 99.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
138.5 °C

実験手順

6.10 g of diethyl (3-trifluoromethyl-2-pyridyl)malonate and 20 ml of dimethyl sulfoxide were mixed. To the mixture was added 1.40 g of sodium chloride and 0.72 g of water. The mixture was stirred for about 20 minutes at an inner temperature of 132 to 145° C. The reaction mixture was allowed to cool to room temperature, then, to the reaction mixture was added water, and extracted with ethyl acetate. The organic layer was washed with saturated brine twice, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure, to obtain 4.64 g of ethyl (3-trifluoromethyl-2-pyridyl)acetate.

後処理

  1. temperatureto cool to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-307c465a4bb94099a99c380e72fe8f83
出典データセット
uspto-grants-2013_12
特許番号
US08598176B2

関連ノート

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