HCID 178470495、化合物 → HCID 178524954、化合物

HRID 132048

反応式

HRID 132048 の反応式
C([O:3][C:4]([C:6]1[C:10]([NH:11][C:12](=[O:21])[C:13]2[C:18]([F:19])=[CH:17][CH:16]=[CH:15][C:14]=2[F:20])=[CH:9][NH:8][N:7]=1)=[O:5])C>[OH-].[Na+].CO>[F:19][C:18]1[CH:17]=[CH:16][CH:15]=[C:14]([F:20])[C:13]=1[C:12]([NH:11][C:10]1[C:6]([C:4]([OH:5])=[O:3])=[N:7][NH:8][CH:9]=1)=[O:21]

参加物

3

反応物 1

HCID 178470495HCID 178470495、化合物

生成物 1

HCID 178524954HCID 178524954、化合物収率 61.7%

試薬・触媒・溶媒 1

HCID 23721981Sodium hydroxide methanol溶媒

実験手順

A mixture of 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid ethyl ester (10.2 g) in 2 M aqueous NaOH/MeOH (1:1, 250 ml) was stirred at ambient temperature for 14 h. Volatile materials were removed in vacuo, water (300 ml) added and the mixture taken to pH 5 using 1M aqueous HCl. The resultant precipitate was collected by filtration and dried through azeotrope with toluene to afford 4-(2,6-difluoro-benzoylamino)-1H-pyrazole-3-carboxylic acid as a pink solid (5.70 g). (LC/MS: Rt 2.33, [M+H]+267.96).

後処理

  1. customVolatile materials were removed in vacuo, water (300 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-2be4b140c6ff4dc68478b5080f7d6a92
出典データセット
uspto-grants-2008_06
特許番号
US07385059B2

関連ノート

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