HCID 178470495, 화합물 → HCID 178524954, 화합물

HRID 20310

반응식

HRID 20310 반응식
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]

참가 물질

3

반응물 1

HCID 178470495HCID 178470495, 화합물

생성물 1

HCID 178524954HCID 178524954, 화합물수율 61.7%

시약·촉매·용매 1

HCID 23721981Sodium hydroxide methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-585e59fc6d6949348d8df84c97e249de
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745638B2

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