Water → 3,4-Dichloro-5-fluoro-2-picoline

HRID 1450065

반응식

HRID 1450065 반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH3:9])[CH:3]=1.C(O[Cl:15])(C)(C)C.O>C(Cl)(Cl)Cl>[Cl:15][C:3]1[C:4]([CH3:9])=[N:5][CH:6]=[C:7]([F:8])[C:2]=1[Cl:1]

참가 물질

5

반응물 3

HCID 962WaterHCID 521297Tert-Butyl hypochloriteHCID 196914104-Chloro-5-fluoro-2-methylpyridine2회

생성물 1

HCID 196912453,4-Dichloro-5-fluoro-2-picoline

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

To 0.87 g (6 mmol) of 4-chloro-5-fluoro-2-picoline, the product of Example 66, in 20 mL of chloroform cooled to -45° C., is added 0.75 mL of t-butylhypochlorite. The reaction mixture is stirred at -45° C. for 2 hours and at 0° C. for 2 hours. The reaction mixture is then poured into water and the resultant aqueous mixture is extracted with methylene chloride. The organic solution is dried over anhydrous magnesium sulfate, filtered, concentrated under reduced pressure and distilled to afford the title compound.

후처리

  1. extractionthe resultant aqueous mixture is extracted with methylene chloride
  2. dry with materialThe organic solution is dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. distillationdistilled

출처 및 근거

ORD 기록
ord-014f44cb018147659fc5b134765083b2
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05599816

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