Acetic Acid → 5-Bromo-1,3-difluoro-2-nitrobenzene

HRID 59931

反応式

HRID 59931 の反応式
[Br:1][C:2]1[CH:8]=[C:7]([F:9])[C:5]([NH2:6])=[C:4]([F:10])[CH:3]=1.[OH2:11].CC(O)=[O:14]>>[Br:1][C:2]1[CH:8]=[C:7]([F:9])[C:5]([N+:6]([O-:14])=[O:11])=[C:4]([F:10])[CH:3]=1

参加物

4

反応物 3

HCID 176Acetic Acid2 回HCID 962Water3 回HCID 6101914-Bromo-2,6-difluoroaniline

生成物 1

HCID 213354875-Bromo-1,3-difluoro-2-nitrobenzene

反応条件

温度
70 °C

実験手順

A solution of 4-bromo-2,6-difluoroaniline (240 mmol) in AcOH (150 mL) was added dropwise to a suspension of NaBO3.4 H2O (325 mmol) in AcOH (450 mL) at 70° C. during 30 min. Another 2080 mmol of NaBO3.4 H2O were added over 5 h to the mixture. During this period the mixture was stirred at 70° C. The mixture was poured into water and extracted with Et2O. The organic layer was combined with another Et2O solution obtained from another reaction using the same conditions described above. The mixture was concentrated. A precipitate was formed and separated by filtration. The filtrate was concentrated to afford the desired product after flash column chromatography (SiO2, petroleum ether).

後処理

  1. extractionextracted with Et2O
  2. customobtained from another reaction
  3. concentrationThe mixture was concentrated
  4. customA precipitate was formed
  5. customseparated by filtration
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-3257fcb39fa44c9aa53c83e4c87efeec
出典データセット
uspto-grants-2016_09
特許番号
US09440929B2

関連ノート

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