Hydrochloric Acid → 3-Chloro-4-methoxysalicylaldehyde

HRID 629379노트

반응식

HRID 629379 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 133437063-Chloro-4-methoxysalicylaldehyde수율 94.7%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 8471Triethylamine용매

반응 조건

온도
70 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b81d52eba97246f68e370c353edec73b
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315458B2

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