Pyridine → 2,3-Dichloro-6-(trifluoromethyl)benzonitrile

HRID 1005483노트

반응식

HRID 1005483 반응식
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[C:3]=1[C:4]([NH2:6])=O.N1C=CC=CC=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O>O1CCOCC1>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:13])[F:14])[C:3]=1[C:4]#[N:6]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 9845Trifluoroacetic anhydrideHCID 154569832,3-Dichloro-6-(trifluoromethyl)benzamide

생성물 1

HCID 109775462,3-Dichloro-6-(trifluoromethyl)benzonitrile수율 94.1%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
8.5 °C

실험 절차

409 g of 2,3-dichloro-6-trifluoromethylbenzamide was dissolved in 2 liters of dioxane, and 263 g of pyridine was further added to the resultant solution. To this solution, 349 g of trifluoroacetic anhydride was added dropwise over 30 minutes while maintaining the temperature from 7 to 10° C. After stirring the solution for 2 hours at 25° C., the reaction mixture was poured into ice water. The precipitated crystals generated were then collected by filtration and were dissolved in ethyl acetate. The solution was then washed with water and saturated saline solution in series and dried over anhydrous magnesium sulfate. The solvent was distilled under reduced pressure, and the crude product obtained was washed with n-hexane and filtered to obtain 358 g of the title compound(mp. 53-54° C.).

후처리

  1. filtrationThe precipitated crystals generated were then collected by filtration
  2. dissolutionwere dissolved in ethyl acetate
  3. washThe solution was then washed with water and saturated saline solution in series
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled under reduced pressure
  6. customthe crude product obtained
  7. washwas washed with n-hexane
  8. filtrationfiltered

출처 및 근거

ORD 기록
ord-707c01b7418d493fa76e149db458bf4f
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06054605

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