Acetic Anhydride → Acetamide, N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-

HRID 34439

反応式

HRID 34439 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH:10]([NH2:12])[CH3:11])=[CH:5][CH:4]=1.[C:13](OC(=O)C)(=[O:15])[CH3:14]>N1C=CC=CC=1>[C:13]([NH:12][C@H:10]([CH3:11])[CH2:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)(=[O:15])[CH3:14]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 31721(+-)-p-Methoxyamphetamine

生成物 1

HCID 11769683Acetamide, N-[(1R)-2-(4-methoxyphenyl)-1-methylethyl]-

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In 6 ml of pyridine was dissolved 1.5 g of (-)-2-(p-methoxyphenyl)-1-methylethylamine ([α]D23 : -30.1° (c=1.2, methanol)), and after adding thereto 3 ml of acetic anhydride, the mixture was allowed to stand at room temperature for 1 hour. After distilling off the solvent, the residue was extracted with ethyl acetate. The ethyl acetate extract was washed with water, and dried over anhydrous sodium sulfate, and the solvent was distilled off and the crude crystals formed were recrystallized from a mixture of n-hexane and benzene to provide 1.8 g of (R)(+)-N-acetyl-2-(p-methoxyphenyl)-1-methylethylamine.

後処理

  1. additionafter adding
  2. distillationAfter distilling off the solvent
  3. extractionthe residue was extracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. washwas washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationthe solvent was distilled off
  8. customthe crude crystals formed
  9. customwere recrystallized from a mixture of n-hexane and benzene

出典と根拠

ORDレコード
ord-7eb9071a423a4cc580b1dc8c119f7b39
出典データセット
uspto-grants-1988_08
特許番号
US04761500

関連ノート

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