4-(4-Aminophenoxy)-N-methylpicolinamide → 4-[4-({[4-bromo-3-(pentafluoro-lambda6-sulfanyl)phenyl]carbamoyl}amino)phenoxy]-N-methylpyridine-2-carboxamide

HRID 1428415ノート

反応式

HRID 1428415 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[O:10])=[CH:4][C:3]=1[S:11]([F:16])([F:15])([F:14])([F:13])[F:12].[NH2:17][C:18]1[CH:34]=[CH:33][C:21]([O:22][C:23]2[CH:28]=[CH:27][N:26]=[C:25]([C:29]([NH:31][CH3:32])=[O:30])[CH:24]=2)=[CH:20][CH:19]=1>C(Cl)Cl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:17][C:18]2[CH:34]=[CH:33][C:21]([O:22][C:23]3[CH:28]=[CH:27][N:26]=[C:25]([C:29]([NH:31][CH3:32])=[O:30])[CH:24]=3)=[CH:20][CH:19]=2)=[O:10])=[CH:4][C:3]=1[S:11]([F:16])([F:12])([F:13])([F:14])[F:15]

参加物

4

反応物 2

HCID 166551294-(4-Aminophenoxy)-N-methylpicolinamideHCID 867012911-Bromo-4-isocyanato-2-(pentafluoro-lambda6-sulfanyl)benzene

生成物 1

HCID 575208864-[4-({[4-bromo-3-(pentafluoro-lambda6-sulfanyl)phenyl]carbamoyl}amino)phenoxy]-N-methylpyridine-2-carboxamide収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The crude 1-bromo-4-isocyanato-2-(pentafluoro-λ6-sulfanyl)benzene obtained above was dissolved in DCM (70 mL). 4-(4-aminophenoxy)-N-methylpicolinamide (1.54 g, 6.34 mmol, 0.8 eq) was added at room temperature under N2. The mixture was stirred at room temperature for about 30 min, a lot of solid precipitated. DCM (30 mL) was added and made the mixture stirred at room temperature for 18 hrs. The solid was filtrated, washed with DCM (50 mL), dried under high vacuum to afford 2.6 g (yield 72%) of the title compound as a white solid.

後処理

  1. customa lot of solid precipitated
  2. additionDCM (30 mL) was added
  3. stirringstirred at room temperature for 18 hrs
  4. filtrationThe solid was filtrated
  5. washwashed with DCM (50 mL)
  6. customdried under high vacuum

出典と根拠

ORDレコード
ord-e4e5ee69e62a499fa5569d359dd8d324
出典データセット
uspto-grants-2015_01
特許番号
US08937088B2

反応ノート

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