関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | N-Methylhomoveratrylamine | HCID 77039 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(3-Chloropropyl)-3,4-dimethoxy-N-methylphenethylamine | HCID 577693 | — |
反応手順
29 ml of 1-bromo-3-chloropropane were dissolved in 300 ml of dimethylformamide and 24 g of potassium carbonate were added to the solution. A solution of 18 g N-[2-(3,4-dimethoxyphenyl)-ethyl]-N-methylamine in 50 ml of dimethylformamide were added to the reaction mixture with stirring, dropwise within 2 hours. Then the reaction mixture was stirred for another hour. Then the salts formed were filtered off. The filtrate was concentrated at a maximum bath temperature of 50° C. The residue was dissolved in 200 ml of 0.5 m citric acid solution and the solution was extracted to remove unreacted bromochloropropane with methyl-tert-butyl ether. The aqueous phase was then made slightly alkaline by adding sodium hydrogen carbonate and extracted several times with ethyl acetate. Then the combined ethyl acetate extracts were dried with magnesium sulfate and concentrated. 21 g of 3-[N-(2-(3,4-dimethoxyphenyl)-ethyl)-N-methylamino]-propyl chloride were obtained as the residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05547967 |
|---|
| 出典データセット | uspto-grants-1996_08 |
|---|
| ORD ID | ord-0177ce9340bb4430bfbc5c730d0f9a69 |
|---|
| 出典メモ | uspto-grants-1996_08 |
|---|