2-Chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene → 2-Chloro-6-difluoromethoxy-3-fluorobenzaldehyde

HRID 2095625노트

반응식

HRID 2095625 반응식
[Cl:1][C:2]1[C:7]([CH:8](OC)[O:9]C)=[C:6]([O:13][CH:14]([F:16])[F:15])[CH:5]=[CH:4][C:3]=1[F:17]>CC(C)=O.O>[Cl:1][C:2]1[C:3]([F:17])=[CH:4][CH:5]=[C:6]([O:13][CH:14]([F:16])[F:15])[C:7]=1[CH:8]=[O:9]

참가 물질

4

반응물 1

HCID 670043632-Chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene

생성물 1

HCID 866593242-Chloro-6-difluoromethoxy-3-fluorobenzaldehyde수율 40%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매2회

실험 절차

To a solution of crude 2-chloro-4-difluoromethoxy-3-dimethoxymethyl-1-fluorobenzene (181 g, 670 mmol) in acetone (650 mL) and water (150 mL) was added Amberlyst-15 resin (540 g, pre-washed with water) and the mixture was stirred using mechanical stirrer for 40 h at RT. The Amberlyst-15 resin was removed by filtration using celite bed on sintered funnel, and the filtrate was evaporated on a rotary evaporator at RT (Note: aldehyde evaporates at higher temperatures under reduced pressure). The residue was purified by column chromatography on silica gel using ethyl acetate/hexanes (5% to 10%) to obtain the title compound (60 g, 40%).

후처리

  1. customfor 40 h
  2. customat RT
  3. customThe Amberlyst-15 resin was removed by filtration
  4. customthe filtrate was evaporated on a rotary evaporator at RT
  5. custom(Note: aldehyde evaporates at higher temperatures under reduced pressure)
  6. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-0e5dd5fc9efe4cd7b3615ab8785f5da5
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445510B2

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