Hydrochloric Acid → N-Acetyl-3,4-dimethoxyphenethylamine

HRID 2253610

反応式

HRID 2253610 の反応式
[CH2:1]([NH2:13])[CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1.[C:14](OC(=O)C)(=[O:16])[CH3:15].Cl>N1C=CC=CC=1>[C:14]([NH:13][CH2:1][CH2:2][C:3]1[CH:12]=[CH:11][C:8]([O:9][CH3:10])=[C:5]([O:6][CH3:7])[CH:4]=1)(=[O:16])[CH3:15]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 8421Homoveratrylamine

生成物 1

HCID 80465N-Acetyl-3,4-dimethoxyphenethylamine

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

After dissolving 5 g of homoveratrylamine in 20 ml of pyridine, 5.6 g of acetic anhydride was added and reacted at 65°-70° C. with stirring for 2 hours. The reaction mixture was poured into 150 ml of ice water and then made weakly acidic by adding 50 ml of a 6N aqueous hydrochloric acid solution. The resultant solution was extracted three times with 50 ml of chloroform. The extracted solution was combined, washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. Ether was added to the residue and precipitated crystals were filtered. N-acetylhomoveratrylamine having a melting point of 101°-102° C. was obtained as colorless crystals. The yield was 5.7 g.

後処理

  1. additionwas added
  2. customreacted at 65°-70° C.
  3. extractionThe resultant solution was extracted three times with 50 ml of chloroform
  4. washwashed with an aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. additionEther was added to the residue
  8. customprecipitated crystals
  9. filtrationwere filtered

出典と根拠

ORDレコード
ord-55778aa0a8aa43f48ab07dc4aa993ad6
出典データセット
uspto-grants-1993_08
特許番号
US05232923

関連ノート

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