関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-(2,3-Epoxypropyl)phthalimide | HCID 21601 | — |
| 反応物 | 2-{[(3,4-Dichlorophenyl)methyl]amino}propan-1-ol | HCID 21962977 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[(cis)-4-(3,4-Dichlorobenzyl)-5-methylmorpholin-2-yl]methanamine | HCID 69507402 | 72.3% |
反応手順
A mixture of Intermediate 4 (0.470 g) and 2-(oxiran-2-ylmethyl)-1H-isoindole-1,3(2H)-dione (0.410 g) was heated at 80° C. under nitrogen for 5 h. The mixture was treated with concentrated sulphuric acid (0.6 ml) then stirred at 150° C. for 42 h. The mixture was treated with water (50 ml) then washed with ethyl acetate (2×50 ml). The dark aqueous phase was basified to ˜pH 11 using 5M aqueous sodium hydroxide then extracted with ethyl acetate (2×50 ml). The combined organic extracts were washed with water and brine, dried (Na2SO4) and concentrated under vacuum to give the title compound as a brown oil (0.42 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07101882B2 |
|---|
| 出典データセット | uspto-grants-2006_09 |
|---|
| ORD ID | ord-bd31778a81e84adb92828a916c1f8897 |
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| 出典メモ | uspto-grants-2006_09 |
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