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2-Oxoadipic acid → Z-2-(2,2-Dimethylcyclopropanecarboxamido)-2-hexenedioic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Oxoadipic acid | HCID 71 | — |
| 反応物 | Methyl isovalerate | HCID 11160 | — |
| 反応物 | 2,2-Dimethylcyclopropanecarboxamide | HCID 574717 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Z-2-(2,2-Dimethylcyclopropanecarboxamido)-2-hexenedioic acid | HCID 13505568 | — |
反応手順
A mixture of 1.0 g. of 2,2-dimethylcyclopropanecarboxamide, 2.4 g. of 2-ketoadipic acid and 25 ml. of methyl isovalerate was heated under reflux for 4 hrs, with removal of H2O by a modified Dean-Stark trap containing molecular sieves (4A). After standing at room temperature overnight, the crystalline precipitate was filtered, washed with ether and recrystallized from ethyl acetate to give 0.23 g. of product, m.p. 163°-165°. The NMR spectrum was consistent with the desired structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04880793 |
| 出典データセット | uspto-grants-1989_11 |
| ORD ID | ord-72ed6172388a4cf08e8f9e36ca625193 |
| 出典メモ | uspto-grants-1989_11 |