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Dimethylformamide → 2-Propynyl 3,4,5-trifluorobenzoate

HRID 2236377
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HRID 2236377 반응식
CN(C=O)C.[F:6][C:7]1[CH:8]=[C:9]([CH:13]=[C:14]([F:17])[C:15]=1[F:16])[C:10]([OH:12])=[O:11].[CH2:18](Br)[C:19]#[CH:20].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C>[F:6][C:7]1[CH:8]=[C:9]([CH:13]=[C:14]([F:17])[C:15]=1[F:16])[C:10]([O:12][CH2:20][C:19]#[CH:18])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 8531543,4,5-Trifluorobenzoic acid

생성물 1

HCID 593017632-Propynyl 3,4,5-trifluorobenzoate수율 98.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To 50 ml of DMF were added 5.0 g of 3,4,5-trifluorobenzoic acid, 4.0 g of propargyl bromide and 4.7 g of potassium carbonate, and the mixture obtained was stirred at room temperature for 30 minutes and then heated with stirring at 80° C. for 1 hour. Then, ethyl acetate was added to the reaction mixture and the mixture was filtered through Celite. Water and dilute hydrochloric acid were added to the filtrate in order and it was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under reduced pressure to obtain 6.0 g of 2-propynyl 3,4,5-trifluorobenzoate represented by the formula:

후처리

  1. customthe mixture obtained
  2. temperatureheated
  3. stirringwith stirring at 80° C. for 1 hour
  4. filtrationthe mixture was filtered through Celite
  5. additionWater and dilute hydrochloric acid were added to the filtrate in order and it
  6. extractionwas extracted with ethyl acetate
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-242fa91751574bceab4fc40f7aff901d
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07714168B2

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