Acetic Acid → 2-(5-Methyl-3-trifluoromethyl-1H-pyrazol-1-yl)phenol

HRID 337332

反応式

HRID 337332 の反応式
Cl.C[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[NH:10][NH2:11].C(O)(=O)C.[F:16][C:17]([F:25])([F:24])[C:18](=O)[CH2:19][C:20](=O)[CH3:21]>COCCO>[CH3:21][C:20]1[N:10]([C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[OH:3])[N:11]=[C:18]([C:17]([F:25])([F:24])[F:16])[CH:19]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 739431,1,1-Trifluoro-2,4-pentanedioneHCID 28494452-Methoxyphenylhydrazine Hydrochloride

生成物 1

HCID 601433782-(5-Methyl-3-trifluoromethyl-1H-pyrazol-1-yl)phenol

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

300 mg of 2-methoxyphenyl hydrazine hydrochloride was dissolved in 1.3 ml of 2-methoxyethanol, and 2.5 ml of acetic acid and 208 μl of 1,1,1-trifluoro-2,4-pentanedione were added and heated at reflux for 1 hour and 40 minutes. The solvent was distilled off under reduced pressure, and 50 ml of ethyl acetate was added, and the organic layer was washed with 50 ml of a saturated sodium bicarbonate solution and 50 ml of saturated saline and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to yield 485.6 mg of the title compound.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1 hour and 40 minutes
  3. distillationThe solvent was distilled off under reduced pressure, and 50 ml of ethyl acetate
  4. additionwas added
  5. washthe organic layer was washed with 50 ml of a saturated sodium bicarbonate solution and 50 ml of saturated saline
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-bbebde9491ce4d5094a0638d627e45e7
出典データセット
uspto-grants-2014_11
特許番号
US08889727B2

関連ノート

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