참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4-Amino-3-Nitrophenol | HCID 3758882 | — |
| 반응물 | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| 용매 | Methyl Ethyl Ketone | HCID 6569 | — |
| 생성물 | 4-(2-(Dimethylamino)ethoxy)-2-nitroaniline | HCID 59349393 | 45% |
반응 단계
To a stirred solution of 4-amino-3-nitro-phenol (1.54 g, 10 mmol) and (2-chloro-ethyl)-dimethyl-amine hydrogen chloride (1.43 g, 10 mmol) in butanone (40 mL) was added Cs2CO3 (10 g, 30 mmol) and NaI (150 g, 1 mmol). The solution was slowly heated to 80° C. over one hour. Then the solution was stirred at 80° C. for 2 hours. The solution was filtered through Celite® and washed with acetone. The solution was evaporated with silica gel and purified by flash chromatography on silica to afford the title compound (1.0 g, yield: 45%) as a brown solid. 1H-NMR (300 MHz, DMSO-d6) δ 7.38 (d, 1H), 7.24 (s, 2H), 7.16 (dd, 2H), 6.99 (d, 1H), 3.98 (t, 214), 2.58 (t, 2H), 2.20 (s, 6H); MS (ESI) 226 [M+H]+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09434697B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-d30e336c6ff44153a84cf56115ad7724 |
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| 출처 메모 | uspto-grants-2016_09 |
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