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Acetonitrile → HCID 86684857、化合物

HRID 238355
ノート
印刷プレビュー

反応式

HRID 238355 の反応式
[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)=[CH:5][CH:4]=[N:3]1.FC(F)(F)S(O[CH2:20][C:21]([F:24])([F:23])[F:22])(=O)=O.C(=O)([O-])[O-].[K+].[K+].C(#N)C>C(Cl)(Cl)Cl>[CH3:1][N:2]1[C:6]([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH2:20][C:21]([F:24])([F:23])[F:22])=[CH:9][CH:8]=2)=[CH:5][CH:4]=[N:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 803662,2,2-Trifluoroethyl trifluoromethanesulfonateHCID 1361148434-(1-methyl-1H-pyrazol-5-yl)phenol

生成物 1

HCID 86684857HCID 86684857、化合物収率 65.9%

試薬・触媒・溶媒 1

HCID 6212Chloroform
溶媒

反応条件

温度
90 °C

実験手順

A mixture of 4-(1-methyl-1H-pyrazol-5-yl)phenol (500 mg), 2,2,2-trifluoroethyl trifluoromethanesulfonate (999 mg), potassium carbonate (793 g) and acetonitrile (5.0 mL) was stirred at 90° C. for 2 hours. Thereafter, the reaction solution was diluted with chloroform, and insoluble matters were then removed by filtration. The filtrate was concentrated under a reduced pressure, and the residue was then purified by column chromatography (silica gel 60N, chloroform:methanol=100:0 to 98:2), so as to obtain the title compound (485 mg) in the form of a light yellow solid.

後処理

  1. customwere then removed by filtration
  2. concentrationThe filtrate was concentrated under a reduced pressure
  3. customthe residue was then purified by column chromatography (silica gel 60N, chloroform:methanol=100:0 to 98:2)

出典と根拠

ORDレコード
ord-3ce85b3801c942ce8bec3fe757138c97
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08642626B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート