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Methyl iodide → 2,4-Dichloro-6-methoxybenzaldehyde

HRID 510637
ノート
印刷プレビュー

反応式

HRID 510637 の反応式
[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([OH:11])[C:3]=1[CH:4]=[O:5].[C:12](=O)([O-])[O-].[K+].[K+].IC>CN(C)C=O.O>[Cl:1][C:2]1[CH:9]=[C:8]([Cl:10])[CH:7]=[C:6]([O:11][CH3:12])[C:3]=1[CH:4]=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 5283902,4-Dichloro-6-hydroxybenzaldehyde

生成物 1

HCID 128028802,4-Dichloro-6-methoxybenzaldehyde収率 97.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of 2,4-dichloro-6-hydroxybenzaldehyde (1.85 g, 9.69 mmol) in N,N-dimethylformamide (20 mL) at ambient temperature was added solid potassium carbonate (1.47 g, 10.7 mmol), and the resulting yellow mixture was stirred at ambient temperature for 30 minutes. Iodomethane (2.42 mL, 38.7 mmol) was added, and the resulting mixture was stirred in an oil bath set to 50° C. for 30 minutes. The mixture was cooled to ambient temperature and diluted with water (200 mL). After stirring for 10 minutes, the precipitate that formed was collected by filtration, washed with water, and dried under vacuum to afford 2,4-dichloro-6-methoxybenzaldehyde as an off-white powder (1.93 g, 97% yield).

後処理

  1. stirringthe resulting mixture was stirred in an oil bath
  2. waitset to 50° C. for 30 minutes
  3. temperatureThe mixture was cooled to ambient temperature
  4. stirringAfter stirring for 10 minutes
  5. customthe precipitate that formed
  6. filtrationwas collected by filtration
  7. washwashed with water
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-5d5c830cfb5d41bd866e2ebcf0c7803c
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096567B2

反応ノート

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