Ethyl 5-methoxy-1-phenyl-1H-pyrazole-4-carboxylate → 5-Methoxy-1-phenyl-1H-pyrazole-4-carboxylic acid

HRID 485679ノート

反応式

HRID 485679 の反応式
C([O:3][C:4]([C:6]1[CH:10]=[N:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]=1[O:17][CH3:18])=[O:5])C>[OH-].[Na+]>[CH3:18][O:17][C:7]1[N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:9]=[CH:10][C:6]=1[C:4]([OH:5])=[O:3]

参加物

3

反応物 1

HCID 15192739Ethyl 5-methoxy-1-phenyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 202690405-Methoxy-1-phenyl-1H-pyrazole-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

The ester prepared as described in (a) above (390 mg, 1.58 mmol) in lN sodium hydroxide (10 ml) was refluxed for 3 hours under nitrogen and then allowed to cool and the solution was washed with ethyl acetate. The aqueous layer was then acidified to pH 2(HCl) whereupon the title compound precipitated out and was filtered and washed with water followed by drying under vacuum (268 mg, 78%), νmax (Nujol) 1680, 1595, 1560 cm-1 δ (D6 -Acetone) 4.24 (3H,s,--OCH3),7.74 (5H,m, phenyl protons), 8.06 (1H,s,C5 pyrazole proton), Found M+ ; 218.0684, C11H10N2O3Requires M,218.0689.

後処理

  1. temperaturewas refluxed for 3 hours under nitrogen
  2. temperatureto cool
  3. washthe solution was washed with ethyl acetate
  4. customprecipitated out
  5. filtrationwas filtered
  6. washwashed with water
  7. dry with materialby drying under vacuum (268 mg, 78%), νmax (Nujol) 1680, 1595, 1560 cm-1 δ (D6 -Acetone) 4.24 (3H,s,--OCH3),7.74 (5H,m, phenyl protons), 8.06 (1H,s,C5 pyrazole proton), Found M+

出典と根拠

ORDレコード
ord-9c9d7428cf314749885d117926dc41c5
出典データセット
uspto-grants-1985_08
特許番号
US04537886

反応ノート

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