Sodium Hydroxide → HCID 71257341、化合物

HRID 710097ノート

反応式

HRID 710097 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][C:3]=1[OH:9].[F:10][C:11]1[CH:19]=[C:18]([S:20]([CH3:23])(=[O:22])=[O:21])[CH:17]=[CH:16][C:12]=1[C:13](O)=O.[OH-].[Na+]>>[Br:8][C:5]1[CH:6]=[CH:7][C:2]2[N:1]=[C:13]([C:12]3[CH:16]=[CH:17][C:18]([S:20]([CH3:23])(=[O:21])=[O:22])=[CH:19][C:11]=3[F:10])[O:9][C:3]=2[CH:4]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 143206052-Amino-5-bromophenolHCID 283559322-Fluoro-4-(methylsulphonyl)benzoic acid

生成物 1

HCID 71257341HCID 71257341、化合物収率 13.2%

反応条件

温度
195 °C

実験手順

2-amino-5-bromophenol (1.72 g, 9.2 mmol) and 2-fluoro-4-(methylsulfonyl)benzoic acid (2 g, 9.2 mmol) were dissolved in polyposphoric acid (30 g). This mixture was heated at 195° C. for three and half hours. Reaction mixture cooled to rt and diluted with ice water (100 ml). Aqueous layer basified with sodium hydroxide pellets to pH 9. Solid that formed was filtered and dried to obtain the crude. Crude was purified by combiflash using a gradient mixture of EtOAc and Petether (1:3) as eluent to afford the titled compound (450 mg) as a dark brown solid.

後処理

  1. customReaction mixture
  2. temperaturecooled to rt
  3. customSolid that formed
  4. filtrationwas filtered
  5. customdried
  6. customto obtain the crude
  7. customCrude was purified by combiflash
  8. additiona gradient mixture of EtOAc and Petether (1:3) as eluent

出典と根拠

ORDレコード
ord-7d032d3f32394817af7e648037b7de09
出典データセット
uspto-grants-2015_11
特許番号
US09181214B2

反応ノート

読み込み中…