참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethylamine | HCID 6341 | — |
| 반응물 | 2-Propanone, 1-(3,4-dimethoxyphenyl)- | HCID 69896 | — |
| 반응물 | Sodium cyanoborohydride | HCID 5003444 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | [2-(3,4-Dimethoxy-phenyl)-1-methyl-ethyl]-ethyl amine | HCID 22061570 | 92% |
반응 단계
A solution of 10 g (51.4 mmol) of 3,4-dimethoxyphenylacetone in 50 mL of methanol was cooled to 0° C. and was treated with 50 mL of 2M solution of ethylamine in methanol. To the reaction mixture 11.5 g (0.183 mmol) of sodium cyanoborohydride was added, and the pH of the reaction mixture was adjusted to 6.5-7 by adding glacial acetic acid. The mixture was allowed to stir at room temperature for 4 days. This was concentrated under reduced pressure, and 150 mL of water was added. The pH of the resulting solution was adjusted to 1 using 6 N HCl. This was extracted with 4×150 mL of ether and the organic layers were discarded. The pH of the aqueous layer was adjusted to 14, and the solution was extracted with 6×100 mL of chloroform. The organic layers were combined, dried (Na2SO4) and concentrated to dryness to give 10.6 g (47.4 mmol, 92%) of 2A as a pale yellow oil (M+H, 224).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07060847B2 |
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| 출처 데이터셋 | uspto-grants-2006_06 |
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| ORD ID | ord-f384dfb7eb134ab891325d8af07c69c5 |
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| 출처 메모 | uspto-grants-2006_06 |
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