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

HRID 1907678

반응식

HRID 1907678 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
138.5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-307c465a4bb94099a99c380e72fe8f83
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598176B2

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