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

HRID 1976521노트

반응식

HRID 1976521 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 21998423N-3,4-methylenedioxyphenyl-N-m-tolylamine수율 40.3%

시약·촉매·용매 2

HCID 24462Copper Sulfate촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e3718fc57c9e4add953c25593165c124
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06228547B1

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