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

HRID 1739648노트

반응식

HRID 1739648 반응식
[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

참가 물질

3

반응물 2

HCID 69990Phenylphosphonic dichlorideHCID 178517592HCID 178517592, 화합물

생성물 1

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

반응 조건

온도
135 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bc1178f62f794614881bac365465cca1
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05968875

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