o-Phenetidine → N-(2-Ethoxyphenyl)-2-methylbenzamide

HRID 1578624

반응식

HRID 1578624 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH2:11]([O:13][C:14]1[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=1[NH2:16])[CH3:12].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>CC(C)=O>[CH2:11]([O:13][C:14]1[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=1[NH:16][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][C:2]=1[CH3:1])[CH3:12]

참가 물질

5

반응물 3

HCID 7203o-PhenetidineHCID 83732-Methylbenzoic acidHCID 14812Phosphorus oxide (P4O10)

생성물 1

HCID 576828N-(2-Ethoxyphenyl)-2-methylbenzamide수율 94.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A 13.6 g (0.1 mol) portion of o-methylbenzoic acid and 13.7 g of o-ethoxyaniline were dissolved in 200 ml of acetone. A 4.7 g (0.033 mol) amount of phosphorus pentoxide was gradually added to the prepared solution at 30°-40°C. After the addition, the reaction mixture was refluxed for 3 hours with stirring. The acetone was removed and the residual product was poured into water and was extracted with toluene. The toluene layer was dried over anhydrous sodium sulfate and the toluene was removed to obtain 24.1 g (94.5%) of a clear pink liquid, having a boiling point of 148°C/0.04 mm Hg and nD20 of 1.5929.

후처리

  1. additionAfter the addition
  2. temperaturethe reaction mixture was refluxed for 3 hours
  3. customThe acetone was removed
  4. additionthe residual product was poured into water
  5. extractionwas extracted with toluene
  6. dry with materialThe toluene layer was dried over anhydrous sodium sulfate
  7. customthe toluene was removed

출처 및 근거

ORD 기록
ord-25e01d54eecf47a7a51dac7c93773065
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937840

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