참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromaleic anhydride | HCID 70728 | — |
| 반응물 | 3-Aminophthalic acid | HCID 79490 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3-(2',3'-Dichloromaleinimidyl)-phthalic anhydride | HCID 54427493 | 58% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04131613 |
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| 출처 데이터셋 | uspto-grants-1978_12 |
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| ORD ID | ord-89c5e3339af441f5ad92c6c3e237f56e |
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| 출처 메모 | uspto-grants-1978_12 |
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