Phenylphosphonic dichloride → 5-Bromo-2-chloro-3-(trifluoromethyl)pyridine

HRID 1739648ノート

反応式

HRID 1739648 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[C:4](O)=[N:5][CH:6]=[C:7]([Br:9])[CH:8]=1.C1(P(Cl)([Cl:21])=O)C=CC=CC=1>>[Cl:21][C:4]1[C:3]([C:2]([F:12])([F:11])[F:1])=[CH:8][C:7]([Br:9])=[CH:6][N:5]=1

参加物

3

反応物 2

HCID 69990Phenylphosphonic dichlorideHCID 178517592HCID 178517592、化合物

生成物 1

HCID 218363025-Bromo-2-chloro-3-(trifluoromethyl)pyridine

反応条件

温度
135 °C

実験手順

The product of Example 5 (11.5 g, 0.048 mol) and phenylphosphoryl dichloride (45 mL) were heated with stirring at 135° C. for four hours and allowed to cool to room temperature. The reaction mixture was poured onto ice (750 g) and allowed to warm to room temperature. The mixture was extracted with dichloromethane (150 mL) and filtered. The organic phase was separated, washed with water and 10% sodium carbonate solution and dried over anhydrous sodium sulphate. Evaporation of the solvent gave 2-chloro-3-trifluoromethyl-5-bromopyridine (11.6 g) as a yellow oil.

後処理

  1. temperatureto cool to room temperature
  2. additionThe reaction mixture was poured onto ice (750 g)
  3. temperatureto warm to room temperature
  4. extractionThe mixture was extracted with dichloromethane (150 mL)
  5. filtrationfiltered
  6. customThe organic phase was separated
  7. washwashed with water and 10% sodium carbonate solution
  8. dry with materialdried over anhydrous sodium sulphate
  9. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-bc1178f62f794614881bac365465cca1
出典データセット
uspto-grants-1999_10
特許番号
US05968875

反応ノート

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