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

HRID 337344노트

반응식

HRID 337344 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85206d9f8af0439a8851e6e3c895e74a
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889727B2

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