HCID 178499177、化合物 → 4-(4-Methylbenzamido)-1H-pyrazole-5-carboxylic acid

HRID 1012112ノート

反応式

HRID 1012112 の反応式
C[O:2][C:3]([C:5]1[C:9]([NH:10][C:11](=[O:19])[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)=[CH:8][NH:7][N:6]=1)=[O:4]>[OH-].[Na+].CO>[CH3:18][C:15]1[CH:14]=[CH:13][C:12]([C:11]([NH:10][C:9]2[C:5]([C:3]([OH:4])=[O:2])=[N:6][NH:7][CH:8]=2)=[O:19])=[CH:17][CH:16]=1

参加物

3

反応物 1

HCID 178499177HCID 178499177、化合物

生成物 1

HCID 1784258454-(4-Methylbenzamido)-1H-pyrazole-5-carboxylic acid収率 75%

試薬・触媒・溶媒 1

HCID 23721981Sodium hydroxide methanol溶媒

実験手順

A mixture of 4-(4-methyl-benzoylamino)-1H-pyrazole-3-carboxylic acid methyl ester (486 mg) in 2 M aqueous NaOH/MeOH (1:1, 50 ml) was stirred at ambient temperature for 14 h. Volatile materials were removed in vacuo, water (100 ml) added and the mixture taken to pH 5 using 2M aqueous HCl. The resultant precipitate was collected by filtration and dried through azeotrope with toluene to afford 4-(4-methyl-benzoylamino)-1H-pyrazole-3-carboxylic acid as a gray solid (345 mg). (LC/MS: Rt 2.35, [M+H]+ 246.09).

後処理

  1. customVolatile materials were removed in vacuo, water (100 ml)
  2. additionadded
  3. filtrationThe resultant precipitate was collected by filtration
  4. dry with materialdried through azeotrope with toluene

出典と根拠

ORDレコード
ord-901c7a0f6d5a4467ad5b1f2978ede50c
出典データセット
uspto-grants-2011_07
特許番号
US07977477B2

反応ノート

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