Sodium Hydroxide → HCID 71257341, 화합물

HRID 710097노트

반응식

HRID 710097 반응식
[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

참가 물질

4

반응물 3

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

생성물 1

HCID 71257341HCID 71257341, 화합물수율 13.2%

반응 조건

온도
195 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d032d3f32394817af7e648037b7de09
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181214B2

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