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Acetic Anhydride → 4-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)phenyl acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | (Z)-4-((4-Hydroxyphenyl)amino)-4-oxobut-2-enoic acid | HCID 1550903 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2,5-Dioxo-2,5-dihydro-1H-pyrrol-1-yl)phenyl acetate | HCID 227684 | 53% |
反応手順
To a three-neck 1 liter reaction vessel equipped with a condenser, a teflon stirring rod and a thermometer, 97 g (0.49 moles) of N-(4-hydroxyphenyl)maleamic acid, 27.7 g (0.38 moles) of sodium acetate and 400 g of acetic anhydride are added and then heated by using silicone oil. When the reaction solution reaches 70° C. for 2 hours with stirring, the solution is poured into a large amount of distilled water and a great amount of precipitates are formed. The precipitate is taken by filtration and washed several times with distilled water to remove acetic acid, followed by recrystallization from ethanol to give the titled compound. Yield 53%. B.P. 155°-158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05262500 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-996413313eac4b079d48530336575859 |
| 出典メモ | uspto-grants-1993_11 |