Hydrochloric Acid → 3-Chloro-4-methoxysalicylaldehyde

HRID 629379ノート

反応式

HRID 629379 の反応式
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:10].[Cl-].[Mg+2].[Cl-].[CH2:14]=[O:15].Cl>ClCCCl.C(N(CC)CC)C>[Cl:1][C:2]1[C:3]([OH:10])=[C:4]([CH:5]=[CH:6][C:7]=1[O:8][CH3:9])[CH:14]=[O:15]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 5360315Magnesium ChlorideHCID 155814712-Chloro-3-methoxyphenol

生成物 1

HCID 133437063-Chloro-4-methoxysalicylaldehyde収率 94.7%

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 8471Triethylamine溶媒

反応条件

温度
70 °C

実験手順

To a solution of 2-chloro-3-methoxyphenol (19.3 g) in 1,2-dichloroethane (150 mL) were added triethylamine (73.7 g), magnesium chloride (57.8 g) and paraformaldehyde (36.5 g), and the mixture was stirred at 70° C. for 4 hr under nitrogen atmosphere. The reaction mixture was poured into 1N hydrochloric acid, and the precipitate was removed by filtration, and washed with dichloromethane. The organic layer was washed with 1N hydrochloric acid and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give the title compound (21.5 g).

後処理

  1. customthe precipitate was removed by filtration
  2. washwashed with dichloromethane
  3. washThe organic layer was washed with 1N hydrochloric acid and saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-b81d52eba97246f68e370c353edec73b
出典データセット
uspto-grants-2016_04
特許番号
US09315458B2

反応ノート

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