Chlorosuccinimide → 4-Bromo-2-chloro-3,5-difluoroaniline

HRID 1270729

反応式

HRID 1270729 の反応式
[Br:1][C:2]1[C:8]([F:9])=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[F:10].C1C(=O)N([Cl:18])C(=O)C1>CN(C=O)C.CCOCC>[Br:1][C:2]1[C:8]([F:9])=[CH:7][C:5]([NH2:6])=[C:4]([Cl:18])[C:3]=1[F:10]

参加物

5

反応物 2

HCID 31398ChlorosuccinimideHCID 27362604-Bromo-3,5-difluoroaniline

生成物 1

HCID 184515214-Bromo-2-chloro-3,5-difluoroaniline

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

4-Bromo-3,5-difluoroaniline (10.5 g, 50.5 mmol) is dissolved in DMF (100 mL). NCS (28.6 g, 50.5 mmol) is added portionwise at room temperature. After 48 hours, the reaction is diluted with Et2O and washed with brine. The separated organic phase is dried (Na2SO4) and concentrated to give an oil. The residue is purified by column chromatography (EtOAc/hexanes) to give 4-bromo-2-chloro-3,5-difluoroaniline.

後処理

  1. washwashed with brine
  2. dry with materialThe separated organic phase is dried (Na2SO4)
  3. concentrationconcentrated
  4. customto give an oil
  5. customThe residue is purified by column chromatography (EtOAc/hexanes)

出典と根拠

ORDレコード
ord-412f43e343fe4ce2a34aeef9f39f29dd
出典データセット
uspto-grants-2007_04
特許番号
US07202364B2

関連ノート

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