関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylmaleic anhydride | HCID 13010 | — |
| 反応物 | 4-Aminocyclohexanol | HCID 81293 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(4-hydroxycyclohexyl)-dimethylmaleimide | HCID 20346782 | 70% |
反応手順
126 g (1 mol) of dimethylmaleic anhydride and 115 g (1 mol) of 4-aminocyclohexanol are warmed, whilst stirring, to 120°-125° C. (internal temperature) for 30 minutes in an oil bath. After cooling to about 20° C., the reaction product is dissolved in 500 ml of methylene chloride and the solution is extracted once with 100 ml of 1 N NaOH, whilst cooling with ice. The reaction product is then washed twice with water and dried over Na2SO4. The solvent is evaporated and the residue is recrystallized from a 1:1 mixture by volume of ethyle acetate and petroleum ether. 155 g (70% of theory) of N-(4-hydroxycyclohexyl)-dimethyl-maleimide are obtained; melting point 109°-111° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04174326 |
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| 出典データセット | uspto-grants-1979_11 |
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| ORD ID | ord-eaf52a7465754a36925234705843f923 |
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| 出典メモ | uspto-grants-1979_11 |
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