Homoveratrylamine → 2-Br-4,5-DMPEA

HRID 623396

反応式

HRID 623396 の反応式
[Br:1]Br.[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH2:13][CH2:14][NH2:15])[CH:8]=[CH:9][C:10]=1[O:11][CH3:12]>C(O)(=O)C>[Br:1][C:8]1[CH:9]=[C:10]([O:11][CH3:12])[C:5]([O:4][CH3:3])=[CH:6][C:7]=1[CH2:13][CH2:14][NH2:15]

参加物

4

反応物 2

HCID 8421HomoveratrylamineHCID 24408Bromine

生成物 1

HCID 8203702-Br-4,5-DMPEA収率 79.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

Bromine (1.1 mL, 22 mmol) in acetic acid (10 mL) was slowly added into a vigorously stirred solution of 2-(3,4-dimethoxyphenyl)ethylamine (3.4 mL, 20 mmol) in 50 mL acetic acid. 2-bromo-4,5-dimethoxylbenzeneethanamine precipitated out after 15 minutes. The mixture was stirred for another two hours, filtered, and washed with dichloromethane 10 mL×3 and petroleum ether 10 mL×3. The resulting solid was taken up in water and the pH was brought to 10 with aqueous KOH solution. Extraction with dichloromethane followed by evaporation of the solvent yielded 4.12 g (78%) 2-Bromo-4,5-dimethoxylbenzeneethanamine. The crude product was dried under dynamic vacuum overnight and used without further purification.

後処理

  1. custom2-bromo-4,5-dimethoxylbenzeneethanamine precipitated out after 15 minutes
  2. filtrationfiltered
  3. washwashed with dichloromethane 10 mL×3 and petroleum ether 10 mL×3
  4. extractionExtraction with dichloromethane
  5. customfollowed by evaporation of the solvent

出典と根拠

ORDレコード
ord-ed05befeaabf42ae8fdc26511a20e7f9
出典データセット
uspto-grants-2016_04
特許番号
US09302990B2

関連ノート

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