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Dimethyl Sulfoxide → Ethyl (3,5-dichloro-2-pyridyl)acetate

HRID 1907680
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인쇄 미리보기

반응식

HRID 1907680 반응식
[Cl:1][C:2]1[C:3]([CH:9](C(OCC)=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.CS(C)=O.[Cl-].[Na+]>O>[Cl:1][C:2]1[C:3]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 57950225HCID 57950225, 화합물

생성물 1

HCID 57447457Ethyl (3,5-dichloro-2-pyridyl)acetate수율 92.2%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
142.5 °C

실험 절차

6.75 g of diethyl (3,5-dichloro-2-pyridyl)malonate and 20 ml of dimethyl sulfoxide were mixed. To the mixture was added 1.57 g of sodium chloride and 0.79 g of water. The mixture was stirred for about 40 minutes at an inner temperature of 135 to 150° C. The mixture was allowed to cool to room temperature, then, water was added to the reaction mixture, 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 4.76 g of ethyl (3,5-dichloro-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-ab465b48078649a28e56d38576c31186
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598176B2

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