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

HRID 1287698

反応式

HRID 1287698 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 576828N-(2-Ethoxyphenyl)-2-methylbenzamide収率 94.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2dacb707b5fd4549a1c468081797601d
出典データセット
uspto-grants-1976_10
特許番号
US03985804

関連ノート

読み込み中…