N-(3-Methylphenyl)acetamide → N-3,4-methylenedioxyphenyl-N-m-tolylamine

HRID 1976521ノート

反応式

HRID 1976521 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][C:9]([CH3:11])=O)[CH:3]=1.[C:12](=[O:15])([O-])[O-:13].[K+].[K+].[OH-].[K+]>S([O-])([O-])(=O)=O.[Cu+2].CO>[CH2:12]1[O:15][C:3]2[CH:4]=[CH:11][C:9]([NH:8][C:4]3[CH:3]=[C:2]([CH3:1])[CH:7]=[CH:6][CH:5]=3)=[CH:1][C:2]=2[O:13]1

参加物

6

反応物 3

HCID 10843N-(3-Methylphenyl)acetamideHCID 11430Potassium CarbonateHCID 14797Potassium Hydroxide

生成物 1

HCID 21998423N-3,4-methylenedioxyphenyl-N-m-tolylamine収率 40.3%

試薬・触媒・溶媒 2

HCID 24462Copper Sulfate触媒HCID 887Methanol溶媒

実験手順

A mixture of 40.0 g (268.1 mol) of m-acetotoluidine, 45.0 g (223.9 mol) of 3,4-bromomethylenedioxybenzene, 8 g (50.1 mol) of copper sulfate, and 31 g (267.7 mmol) of potassium carbonate was reacted in the same manner as in Example 5 (2) to obtain a crude reaction product. A mixture of this crude product, 50 g (757.4 mmol) of 85% KOH, and 200 ml of methanol was refluxed overnight and then concentrated. Water was added thereto. The resultant mixture was extracted with toluene twice. The toluene phase was washed with water three times, dried, and then concentrated. The residue was distilled under vacuum to obtain 24.51 g of N-3,4-methylenedioxyphenyl-N-m-tolylamine.

後処理

  1. customto obtain a crude
  2. customreaction product
  3. temperaturewas refluxed overnight
  4. concentrationconcentrated
  5. additionWater was added
  6. extractionThe resultant mixture was extracted with toluene twice
  7. washThe toluene phase was washed with water three times
  8. customdried
  9. concentrationconcentrated
  10. distillationThe residue was distilled under vacuum

出典と根拠

ORDレコード
ord-e3718fc57c9e4add953c25593165c124
出典データセット
uspto-grants-2001_05
特許番号
US06228547B1

反応ノート

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