関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Chloro-2-fluoro-4-iodopyridine | HCID 21865336 | — |
| 反応物 | HCID 178511674 | HCID 178511674 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 178511614 | HCID 178511614 | 85.8% |
反応手順
A mixture of 5-chloro-2-fluoro-4-iodopyridine (1000 mg, 3.88 mmol), DMSO (7 ml), and trans-cyclohexane-1,4-diamine (2661 mg, 23.31 mmol) reaction mixture was stirred at about 85° C. for 2 hours, followed by LCMS. The crude reaction mixture then was mixed with 5 ml DMSO, filtered and purified by prep LC. After lyapholization, 1.17 grams of the title compound was obtained as a TFA salt. LCMS (m/z): 352.1 (MH+), retention time=0.50 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08778951B2 |
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| 出典データセット | uspto-grants-2014_07 |
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| ORD ID | ord-418e9cc1774e42ad9f4d8e034df7f7a2 |
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| 出典メモ | uspto-grants-2014_07 |
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