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Homoveratrylamine → 2-Br-4,5-DMPEA
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Homoveratrylamine | HCID 8421 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Br-4,5-DMPEA | HCID 820370 | 79.2% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09302990B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-ed05befeaabf42ae8fdc26511a20e7f9 |
| 出典メモ | uspto-grants-2016_04 |