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

HRID 2095625ノート

反応式

HRID 2095625 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

HCID 866593242-Chloro-6-difluoromethoxy-3-fluorobenzaldehyde収率 40%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0e5dd5fc9efe4cd7b3615ab8785f5da5
出典データセット
uspto-grants-2013_05
特許番号
US08445510B2

反応ノート

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