Homoveratrylamine → 2-Br-4,5-DMPEA

HRID 623396

반응식

HRID 623396 반응식
[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]

참가 물질

4

반응물 2

HCID 8421HomoveratrylamineHCID 24408Bromine

생성물 1

HCID 8203702-Br-4,5-DMPEA수율 79.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ed05befeaabf42ae8fdc26511a20e7f9
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09302990B2

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