Potassium Hydroxide → 2-(3,5-Dimethyl-1H-pyrazol-1-yl)benzene-1,3-diol

HRID 337344ノート

反応式

HRID 337344 の反応式
CC1C=CC(S([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([OH:18])[C:13]=2[N:19]2[C:23]([CH3:24])=[CH:22][C:21]([CH3:25])=[N:20]2)(=O)=O)=CC=1.[OH-].[K+]>C(O)C.O>[CH3:25][C:21]1[CH:22]=[C:23]([CH3:24])[N:19]([C:13]2[C:14]([OH:18])=[CH:15][CH:16]=[CH:17][C:12]=2[OH:11])[N:20]=1

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 867032542-(3,5-Dimethyl-1H-pyrazol-1-yl)-3-hydroxyphenyl 4-methylbenzenesulfonate

生成物 1

HCID 601438812-(3,5-Dimethyl-1H-pyrazol-1-yl)benzene-1,3-diol収率 58.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

To 62 mg of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-3-hydroxyphenyl 4-methylbenzene sulfonate was added a solution in which 97 mg of potassium hydroxide was dissolved in 1.5 ml of ethanol and 1.5 ml of water, and heated at reflux for 3.5 hours. To the reaction mixture, 20 ml of water was added, and extracted with 20 ml of ethyl acetate. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and purified using preparative thin-layer silica gel column chromatography (hexane:ethyl acetate=1:1) to yield 20.8 mg of the title compound.

後処理

  1. temperatureat reflux for 3.5 hours
  2. extractionextracted with 20 ml of ethyl acetate
  3. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. custompurified

出典と根拠

ORDレコード
ord-85206d9f8af0439a8851e6e3c895e74a
出典データセット
uspto-grants-2014_11
特許番号
US08889727B2

反応ノート

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