3-[4-(4-Cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid methyl ester → 3-[4-(4-Cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid

HRID 1468177ノート

反応式

HRID 1468177 の反応式
C[O:2][C:3](=[O:24])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([CH2:10][N:11]2[CH:15]=[C:14]([C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[CH:13]=[N:12]2)[CH:5]=1>CO.O>[C:22]([C:19]1[CH:18]=[CH:17][C:16]([C:14]2[CH:13]=[N:12][N:11]([CH2:10][C:6]3[CH:5]=[C:4]([CH:9]=[CH:8][CH:7]=3)[C:3]([OH:24])=[O:2])[CH:15]=2)=[CH:21][CH:20]=1)#[N:23]

参加物

3

反応物 1

HCID 675085333-[4-(4-Cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid methyl ester

生成物 1

HCID 675082023-[4-(4-Cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid収率 82.4%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

Add LiOH monohydrate (0.03 g, 0.8 mmol) to a suspension of 3-[4-(4-cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid methyl ester (0.2 g, 0.6 mmol) in 5 mL of a 4:1 MeOH-water mixture and stir the reaction at room temperature overnight. Concentrate the reaction to remove most of the MeOH, dilute with additional H2O and neutralize by the addition of 1 N aqueous HCl. Isolate the resulting solid by filtration and dry to afford 0.15 g, 71% yield of 3-[4-(4-cyano-phenyl)-pyrazol-1-ylmethyl]-benzoic acid.

後処理

  1. customthe reaction at room temperature overnight
  2. concentrationConcentrate
  3. customthe reaction
  4. customto remove most of the MeOH
  5. additiondilute with additional H2O and neutralize by the addition of 1 N aqueous HCl
  6. customIsolate the resulting solid
  7. filtrationby filtration
  8. customdry

出典と根拠

ORDレコード
ord-e61d724ed5f14b7782df7400fb053c02
出典データセット
uspto-grants-2015_04
特許番号
US09000154B2

反応ノート

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