참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Methoxypropylamine | HCID 1672 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-(2-Phenylpyrimidin-5-yl)thiazole-4-carboxylic acid | HCID 59252475 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | N-(3-methoxypropyl)-2-(2-phenylpyrimidin-5-yl)thiazole-4-carboxamide | HCID 59252401 | — |
반응 단계
To a solution consisting of 2-(2-phenylpyrimidin-5-yl)thiazole-4-carboxylic acid (Example 63, 80 mg, 0.28 mmol) in dichloromethane (10 mL) was added EDAC (75 mg, 0.39 mmol) and HOBt (53 mg, 0.39 mmol) at 0° C. To this mixture was added 3-methoxypropylamine (25 mg, 0.28 mmol) dissolved in dichloromethane (2 mL) and diisopropylethylamine (0.52 mL, 390 mg, 3.0 mmol). The solution was allowed to reach room temperature and stirred for 18 hours. The solvent was evaporated away under reduced pressure and the residue was purified by silica gel flash chromatography (1:1 v/v hexane-ethyl acetate to 100% ethyl acetate gradient) through a 25-g Silicycle® flash silica cartridge. The title compound was obtained as an off-white solid (21 mg, 21% yield); Rf 0.70 with 4:1 v/v ethyl acetate-hexane; melting point 134-136° C.; 1H-NMR (300 MHz; CDCl3) δ 9.31 (s, 2H), 8.52 (dd, 2H), 8.20 (s, 1H), 7.88 (br t, 1H), 7.53 (m, 3H), 3.62 (t, 2H); 3.59 (t, 2H); 3.41 (s, 3H), 1.96 (m, 2H); MS (ESI+) m/z 355 (M+1); H-PGDS FPBA IC50: 3.4 μM.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536185B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-ad6c6539b9aa414784569152efc8236a |
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| 출처 메모 | uspto-grants-2013_09 |
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