(2-Amino-5-bromophenyl)(2-fluorophenyl)methanone → 5-Bromo-2-(3,4-dimethoxyphenylsulfonamido)-2'-fluorobenzophenone

HRID 1608854ノート

反応式

HRID 1608854 の反応式
[NH2:1][C:2]1[CH:16]=[CH:15][C:14]([Br:17])=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5].[CH3:18][O:19][C:20]1[CH:21]=[C:22]([S:28](Cl)(=[O:30])=[O:29])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]>N1C=CC=CC=1>[Br:17][C:14]1[CH:15]=[CH:16][C:2]([NH:1][S:28]([C:22]2[CH:23]=[CH:24][C:25]([O:26][CH3:27])=[C:20]([O:19][CH3:18])[CH:21]=2)(=[O:30])=[O:29])=[C:3]([CH:13]=1)[C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[F:12])=[O:5]

参加物

4

反応物 2

HCID 73865(2-Amino-5-bromophenyl)(2-fluorophenyl)methanoneHCID 27341833,4-Dimethoxybenzenesulfonyl chloride

生成物 1

HCID 233687105-Bromo-2-(3,4-dimethoxyphenylsulfonamido)-2'-fluorobenzophenone

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

20 g of 2-amino-5-bromo-2'-fluorobenzophenone are heated at 85° C. for 48 hours in 120 ml of dry pyridine in the presence of 20 g of 3,4-dimethoxyphenylsulfonyl chloride. The mixture is cooled, poured into ice-cold water, the solid is filtered off, the solid is extracted with AcOEt, the organic phase is washed with water, a solution of hydrochloric acid (1N), water and then saline water. After drying over magnesium sulfate and evaporating the solvent under vacuum, a solid is obtained which is recrystallized from DCM/isopropyl ether.

後処理

  1. temperatureThe mixture is cooled
  2. additionpoured into ice-cold water
  3. filtrationthe solid is filtered off
  4. extractionthe solid is extracted with AcOEt
  5. washthe organic phase is washed with water
  6. dry with materialAfter drying over magnesium sulfate
  7. customevaporating the solvent under vacuum
  8. customa solid is obtained which
  9. customis recrystallized from DCM/isopropyl ether

出典と根拠

ORDレコード
ord-44acd343b15e467caa518c10ed8bfb7f
出典データセット
uspto-grants-1995_03
特許番号
US05397801

反応ノート

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