関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromaleic anhydride | HCID 70728 | — |
| 反応物 | 3-Aminophthalic acid | HCID 79490 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3-(2',3'-Dichloromaleinimidyl)-phthalic anhydride | HCID 54427493 | 58% |
反応手順
20 g (0.12 mol) of 2,3-dichloromaleic anhydride are added to a solution of 18.1 g (0.1 mol) of 3-aminophthalic acid in 90 ml of dioxane. The reaction mixture is stirred to 20°-30° C., whereupon a clear solution is produced over the course of approx. 30 minutes. The dioxane is then distilled off in vacuo (20 mm Hg) and the oil which remains is warmed to 130° C. After 3 hours, the crystalline mass is cooled to 50° C. and mixed with 100 ml of ethyl acetate. The reaction product is filtered off at 10° C. and dried in vacuo at 80° C. 18.1 g (58% of theory) of crystalline 3-(2',3'-dichloromaleinimidyl)-phthalic anhydride are obtained, melting at 229°-230° C. after recrystallisation from anhydrous acetic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04131613 |
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| 出典データセット | uspto-grants-1978_12 |
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| ORD ID | ord-89c5e3339af441f5ad92c6c3e237f56e |
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| 出典メモ | uspto-grants-1978_12 |
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