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

HRID 915381

反応式

HRID 915381 の反応式
[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

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 178519318HCID 178519318、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8c9feac1e29e478b81b2fcccc84a8349
出典データセット
uspto-grants-2007_09
特許番号
US07265149B2

関連ノート

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