Sodium Hydroxide → 3,4,5-Trichloro-6-fluoro-2-pyridone

HRID 461580노트

반응식

HRID 461580 반응식
[Cl:1][C:2]1[C:3](F)=[N:4][C:5]([F:10])=[C:6]([Cl:9])[C:7]=1[Cl:8].[OH-:12].[Na+]>O1CCOCC1.O>[Cl:1][C:2]1[C:3](=[O:12])[NH:4][C:5]([F:10])=[C:6]([Cl:9])[C:7]=1[Cl:8]

참가 물질

5

반응물 2

HCID 14798Sodium Hydroxide3회HCID 6453828Pyridine, 3,4,5-trichloro-2,6-difluoro-

생성물 1

HCID 213914073,4,5-Trichloro-6-fluoro-2-pyridone

시약·촉매·용매 2

HCID 962Water용매3회HCID 312751,4-Dioxane용매

실험 절차

A solution of 3,4,5-trichlorodifluoropyridine (21.8 g.) in dioxan (220 ml.) was refluxed with a solution of sodium hydroxide (8 g.) in water (40 ml.). After 2 hours a further 8 g. of sodium hydroxide in water (40 ml.) was added (4 molar equivalents of sodium hydroxide in toto). After a further 2 hours, water was added to produce a homogeneous solution which was acidified to precipitate the product (17.6 g., m.p. 170°-4°). After initial purification by charcoal and silica gel column, crystallisation from benzene gave 3,4,5-trichloro-6-fluoro-2-pyridone, m.p. 172°-6°(11.8 g.), having a pale yellow colour. After vacuum sublimation at 100°-120°, the white microcrystals melted at 173°-4° (10.65 g/.).

후처리

  1. waitAfter a further 2 hours
  2. customto produce a homogeneous solution which
  3. customto precipitate the product (17.6 g., m.p. 170°-4°)
  4. customAfter initial purification
  5. customby charcoal and silica gel column, crystallisation from benzene

출처 및 근거

ORD 기록
ord-a913e5eee14e4872bfb493cbb5d08548
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04063926

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