Bis(2-chloro-4-fluoro-5-nitrophenyl)carbonate → Bis(2-chloro-4-fluoro-5-aminophenyl)carbonate

HRID 742429ノート

反応式

HRID 742429 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:9]([O-])=O)=[CH:4][C:3]=1[O:12][C:13](=[O:26])[O:14][C:15]1[CH:20]=[C:19]([N+:21]([O-])=O)[C:18]([F:24])=[CH:17][C:16]=1[Cl:25].[H][H]>C1(C)C=CC=CC=1.[Pd]>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([NH2:9])=[CH:4][C:3]=1[O:12][C:13](=[O:26])[O:14][C:15]1[CH:20]=[C:19]([NH2:21])[C:18]([F:24])=[CH:17][C:16]=1[Cl:25]

参加物

5

反応物 2

HCID 14534132Bis(2-chloro-4-fluoro-5-nitrophenyl)carbonateHCID 178418361HCID 178418361、化合物3 回

生成物 1

HCID 15766649Bis(2-chloro-4-fluoro-5-aminophenyl)carbonate収率 99.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

実験手順

Bis(2-chloro-4-fluoro-5-nitrophenyl)carbonate (1.2 Kg, 2.9 mol), toluene (7 liters) as a solvent and 5% Pd/C (200 g) as a catalyst were placed in a 10L three-necked flask equipped with a stirrer, and hydrogen gas was introduced while vigorously stirring. Heat generated as the reaction proceeded, and the reaction temperature was maintained at 60° to 70° C. by introducing hydrogen at such a rate that the hydrogen gas did not discharge from the system. After completion of the reaction, the reaction mixture was heated (60°-70° C.), and the catalyst was separated by filtration. The organic layer of the filtrate was separated and dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and the solvent was distilled off under reduced pressure to obtain bis(2-chloro-4-fluoro-5-aminophenyl)carbonate as a white solid (1.01Kg, 2.89 mol, 99.6% yield).

後処理

  1. customequipped with a stirrer
  2. temperatureHeat
  3. temperaturethe reaction temperature was maintained at 60° to 70° C.
  4. customAfter completion of the reaction
  5. temperaturethe reaction mixture was heated (60°-70° C.)
  6. customthe catalyst was separated by filtration
  7. customThe organic layer of the filtrate was separated
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customThe drying agent was separated by filtration
  10. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-6147161dc49b45348c4b31288a7f0a3d
出典データセット
uspto-grants-1996_09
特許番号
US05554581

反応ノート

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