関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | HCID 59452727 | HCID 59452727 | — |
| 溶媒 | Dichloromethane ethyl acetate methanol | HCID 21901258 | — |
| 生成物 | HCID 59452788 | HCID 59452788 | 76.1% |
反応手順
1-[2-methyl-5-(methyloxy)-4-nitrophenyl]-4-(methylsulfonyl)piperazine (0.87 g, 2.64 mmol) was placed in a 100 mL high pressure vessel and dissolved in 60 mL of 1 to 1 to 1 EtOAc/MeOH/DCM. 5 wt % Platinum(sulfided)/C (1.03 g, 0.26 mmol) was added followed quickly by a rubber septum. The vessel was evacuated and filled with N2 six times to remove any oxygen. The vessel was then pressurized with H2 (60 psi). The solution stirred overnight. The next morning the vessel was evacuated and filled with N2 six times to remove any H2. The solution was filtered through celite and evaporated to afford the title compound of step B (0.602 g, 2.01 mmol, 76%). 1H NMR (400 MHz, DMSO-d6) δ ppm 6.58 (s, 1H), 6.43 (s, 1H), 4.44 (s, 2H), 3.69 (s, 3H), 3.15-3.23 (m, 4H), 2.90 (s, 3H), 2.77-2.83 (m, 4H), 2.06 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08093239B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-d32f5ea37b6548bda6f89e4ac3b28985 |
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| 出典メモ | uspto-grants-2012_01 |
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