Methyl iodide → 1,2-Dichloro-3,4-dimethoxybenzene

HRID 1074182

反応式

HRID 1074182 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[C:4]([OH:9])[C:3]=1O.[C:11](=[O:14])([O-])[O-].[K+].[K+].[CH3:17]I>CC(C)=O>[Cl:8][C:7]1[CH:6]=[CH:5][C:4]([O:9][CH3:17])=[C:3]([O:14][CH3:11])[C:2]=1[Cl:1]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 198773,4-Dichlorocatechol

生成物 1

HCID 560611,2-Dichloro-3,4-dimethoxybenzene収率 91.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A suspension of 104 g of 3,4-dichloro-1,2-benzenediol, 240 g of potassium carbonate and 354 g of methyl iodide in 2 litters of acetone is refluxed for 2 hours. The reaction mixture is filtered and washed with acetone. The filtrate and the washings are combined and evaporated to remove solvent. Water is added to the residue and the mixture is extracted with ethyl acetate. The extract is washed with water, dried and evaporated to remove solvent. The residue is distilled under reduced pressure to give 110.5 g of 1,2-dichloro-3,4-dimethoxybenzene.

後処理

  1. filtrationThe reaction mixture is filtered
  2. washwashed with acetone
  3. customevaporated
  4. customto remove solvent
  5. additionWater is added to the residue
  6. extractionthe mixture is extracted with ethyl acetate
  7. washThe extract is washed with water
  8. customdried
  9. customevaporated
  10. customto remove solvent
  11. distillationThe residue is distilled under reduced pressure

出典と根拠

ORDレコード
ord-5fd3bd26e90d4db59d9902693ff33f37
出典データセット
uspto-grants-1990_11
特許番号
US04973600

関連ノート

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