Trifluoroacetic acid → HCID 23149183, 화합물

HRID 1983054노트

반응식

HRID 1983054 반응식
[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][N:7](CC2C=CC(OC)=CC=2)[CH:8]=1.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+]>>[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][NH:7][CH:8]=1

참가 물질

4

반응물 3

HCID 6422Trifluoroacetic acidHCID 516892Sodium BicarbonateHCID 57712427HCID 57712427, 화합물

생성물 1

HCID 23149183HCID 23149183, 화합물수율 29.2%

반응 조건

온도
65 °C

실험 절차

1.04 g of 4-{[dichlorofluoromethyl]thio}-1-(4-methoxybenzyl)-1H-pyrazole was dissolved to 6 ml of trifluoroacetic acid, followed by stirring at 65° C. for 3 hours. After the reaction mixture was cooled to room temperature, it was added to saturated aqueous solution of sodium hydrogen carbonate. The mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.19 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole.

후처리

  1. temperatureAfter the reaction mixture was cooled to room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-131e44626a8d4a1390e459e58d5a8591
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

반응 노트

불러오는 중…