関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Dimethylmaleic anhydride | HCID 13010 | — |
| 反応物 | Disodium 3,5-diaminophthalate | HCID 20346778 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3,5-Bis-(dimethylmaleimidyl)-phthalic anhydride | HCID 53973683 | 115.7% |
反応手順
7.20 g (0.039 mol) of disodium 3,5-diaminophthalate, dissolved in 200 ml of water, are added to a solution of 8.82 g (0.078 mol) of dimethylmaleic anhydride in 80 ml of toluene. This mixture is boiled under reflux for 1 hour. It is then evaporated to dryness in a rotary evaporator, the residue is dissolved, at 90° C., in 100 ml of N,N-dimethylacetamide and 50 ml of water and the solution is rendered acid to Congo Blue with 10% strength hydrochloric acid. After cooling, the slurry-like mixture is filtered and the residue is rinsed with acetone and then dried in vacuo at 80° C. The dry residue is then suspended in 100 ml of acetic anhydride and this mixture is warmed to about 100° C. for 1 hour. It is then evaporated to dryness and the residue is recrystallised from 1,2-dichlorobenzene. 8.9 g (69% of theory) of 3,5-bis-(dimethylmaleimidyl)-phthalic anhydride are obtained; colour: light brownish; melting point 298° C. (decomposition).
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-31ac854078dd47d5a35fc2cb1eaee9ab |
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| 出典メモ | uspto-grants-1979_11 |
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