関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone | HCID 180 | — |
| 反応物 | Trifluoromethanesulfonic acid | HCID 62406 | — |
| 反応物 | 1,3-Bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl cyanoacetate | HCID 53827082 | — |
| 生成物 | 1,3-Bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl 2-cyano-3,3-dimethylacrylate | HCID 54399067 | 86% |
反応手順
1 g of trifluoromethanesulfonic acid was added to a solution of 55.2 g (0.1 mole) of 1,3-bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl cyanoacetate in 300 ml of acetone, and the solution was heated for 3 hours at a temperature of 56° C. After cooling to room temperature, the resulting crystalline precipitate was filtered off with suction and recrystallized from acetone. After drying, 51 g (86 percent of theory) of 1,3-bis-(4-benzoyl-3-hydroxyphenoxy)-prop-2-yl 2-cyano-3,3-dimethylacrylate were obtained in the form of colorless crystals having a melting point of 145° to 147° C. and a purity of 99 percent (HPLC). The structure of the compound obtained was confirmed by UV, IR and NMR spectra.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04824892 |
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| 出典データセット | uspto-grants-1989_04 |
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| ORD ID | ord-d1be10188bd749ccb265edf5ad1c132b |
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| 出典メモ | uspto-grants-1989_04 |
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