참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 3-Amino-1-propanol | HCID 9086 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Benzyl-2-(dimethylamino)-1-(4-fluorophenyl)butan-1-one | HCID 19360599 | — |
| 용매 | Dimethylacetamide | HCID 31374 | — |
| 생성물 | HCID 19360612 | HCID 19360612 | — |
반응 단계
15.0 g (0.050 mol) of 1-(4-fluorophenyl)-2-dimethylamino-2-benzyl-butan-1-one and 26.3 g (0.35 mol) of 3-amino-1-propanol are dissolved in 30 ml of dry dimethylacetamide, and the solution is heated up to 150° C. together with 13.8 g (0.1 mol) of potassium carbonate, and stirred overnight (about 12 h). After the solution is cooled down, it is poured into 300 ml of water and extracted with ethyl acetate. The organic phase is washed with water and saturated sodium chloride solution, and dried over MgSO4. After distilling off the ethyl acetate, the residue is purified by means of column chromatography on silica gel with ethyl acetate-hexane (1:1) as an eluent, and an oily product is obtained. The structure is confirmed by the 1H-NMR spectrum (CDCl3): δ [ppm]: 0.68 (t, 3H), 1.52 (br, 1H), 1.82-1.94 (m, 3H), 2.00-2.07 (m, 1H), 2.35 (s, 6H), 3.17 (d, 1H), 3.20 (d, 1H), 3.32-3.37 (m, 2H), 3.81-3.85 (m, 2H), 4.42 (br, 1H), 6.52 (d, 2H), 7.14-7.28 (m, 5H), 8.32 (d, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06022906 |
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| 출처 데이터셋 | uspto-grants-2000_02 |
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| ORD ID | ord-3ce85f544e7544c6bee7c395f9f17ae8 |
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| 출처 메모 | uspto-grants-2000_02 |
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