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

HRID 337332

반응식

HRID 337332 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 80192-Methoxyethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bbebde9491ce4d5094a0638d627e45e7
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889727B2

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