Thionyl Chloride → 3-Chloromethyl-5-(4-trifluoromethyl-phenyl)-1H-pyrazole

HRID 915381

반응식

HRID 915381 반응식
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[NH:13][N:12]=[C:11]([CH2:14]O)[CH:10]=2)=[CH:5][CH:4]=1.S(Cl)([Cl:20])=O>C(Cl)(Cl)Cl>[Cl:20][CH2:14][C:11]1[CH:10]=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([C:2]([F:17])([F:16])[F:1])=[CH:4][CH:5]=2)[NH:13][N:12]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 178519318HCID 178519318, 화합물

생성물 1

HCID 1785061113-Chloromethyl-5-(4-trifluoromethyl-phenyl)-1H-pyrazole수율 97.1%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
60 °C

실험 절차

To a solution of [5-(4-trifluoromethyl-phenyl)-1H-pyrazol-3-yl]-methanol (40 mg, 0.17 mmol) in chloroform (4 ml) was added thionyl chloride (0.34 ml, 4.7 mmol) at 0° C. under an argon atmosphere. The solution was stirred at 40° C. for 2 h and at 60° C. for 10 min. The mixture was poured onto ice water/aqueous NaHCO3 1/1, extracted two times with dichloromethane and the combinded extracts were dried over sodium sulfate. Evaporation of the solvent under reduced pressure gave 43 mg (0.165 mmol, 97%) of the title compound as white crystals.

후처리

  1. extractionextracted two times with dichloromethane
  2. dry with materialthe combinded extracts were dried over sodium sulfate
  3. customEvaporation of the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-8c9feac1e29e478b81b2fcccc84a8349
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265149B2

연결된 노트

불러오는 중…