Trifluoroacetic acid → 5-Amino-4-[3-(carboxymethyloxy)benzoyl]-1-(4-fluorophenyl)pyrazole

HRID 489843ノート

反応式

HRID 489843 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14](=[O:30])[C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][C:23]([O:25]C(C)(C)C)=[O:24])[CH:16]=1.FC(F)(F)C(O)=O>C(Cl)Cl>[NH2:1][C:2]1[N:6]([C:7]2[CH:8]=[CH:9][C:10]([F:13])=[CH:11][CH:12]=2)[N:5]=[CH:4][C:3]=1[C:14](=[O:30])[C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH2:22][C:23]([OH:25])=[O:24])[CH:16]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 98228865-Amino-4-[3-(tert-butoxycarbonylmethyloxy)benzoyl]-1-(4-fluorophenyl)pyrazole

生成物 1

HCID 98849735-Amino-4-[3-(carboxymethyloxy)benzoyl]-1-(4-fluorophenyl)pyrazole収率 68.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 5-amino-4-[3-(tert-butoxycarbonylmethyloxy)benzoyl]-1-(4-fluorophenyl)pyrazole (1.0 g, 3.3 mmol) and trifluoroacetic acid (15 ml, 194 mmol) in methylene chloride (15 ml) was stirred overnight at room temperature. The organics were removed in vacuo and the residue was dissolved in toluene. The solution was concentrated and the residue was triturated between ethyl acetate and hexane to give 5-amino-4-[3-(carboxymethyloxy)benzoyl]-1-(4-fluorophenyl)pyrazole (0.8 g) as a solid.

後処理

  1. customThe organics were removed in vacuo
  2. dissolutionthe residue was dissolved in toluene
  3. concentrationThe solution was concentrated
  4. customthe residue was triturated between ethyl acetate and hexane

出典と根拠

ORDレコード
ord-89c273954dd84da6b15ee5301da0fa51
出典データセット
uspto-grants-2005_12
特許番号
US06979693B2

反応ノート

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