Hydrogen Bromide → 3-(2-Amino-2-phenylethyl)phenol

HRID 971999ノート

反応式

HRID 971999 の反応式
Cl.C[O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH:11]([NH2:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:7]=[CH:8][CH:9]=1.Br>C(O)(=O)C>[OH:3][C:4]1[CH:5]=[C:6]([CH2:10][CH:11]([NH2:18])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:7]=[CH:8][CH:9]=1

参加物

4

実験手順

A mixture of dl-2-(3-methoxyphenyl)-1-phenylethylamine hydrochloride (11.3 g), 48% hydrobromic acid (100 ml) and glacial acetic acid (30 ml) is refluxed for 4 hours. After the reaction, the solvent is distilled off. To the residue is added water and the mixture is made alkaline with ammonia and extracted with chloroform. The chloroform layer is dried over anhydrous potassium carbonate and the solvent is distilled off. To the residue is added ether. The precipitated crystals are separated by filtration and recrystallized from ethanol-ethyl acetate to give the desired compound (7.3 g), melting point: 179°-181° C.

後処理

  1. temperatureis refluxed for 4 hours
  2. customAfter the reaction
  3. distillationthe solvent is distilled off
  4. additionTo the residue is added water
  5. extractionextracted with chloroform
  6. dry with materialThe chloroform layer is dried over anhydrous potassium carbonate
  7. distillationthe solvent is distilled off
  8. additionTo the residue is added ether
  9. customThe precipitated crystals are separated by filtration
  10. customrecrystallized from ethanol-ethyl acetate

出典と根拠

ORDレコード
ord-22ae2fde10ee4a859bcff85fcaa8f799
出典データセット
uspto-grants-1979_07
特許番号
US04162316

反応ノート

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