참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Bromo-3-chloropropane | HCID 8006 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | N-Methylhomoveratrylamine | HCID 77039 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(3-Chloropropyl)-3,4-dimethoxy-N-methylphenethylamine | HCID 577693 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05547967 |
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| 출처 데이터셋 | uspto-grants-1996_08 |
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| ORD ID | ord-0177ce9340bb4430bfbc5c730d0f9a69 |
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| 출처 메모 | uspto-grants-1996_08 |
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