関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Diphenyl diselenide | HCID 15460 | — |
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | Phthalimide potassium salt | HCID 24194345 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-2-(2-Furanyl)propenylphthalimide | HCID 53798517 | 299.9% |
反応手順
To a solution of 8.35 g (0.077 mole) of the olefin of Step A in 310 ml of DMF was added 12.37 g (0.093 mole) of N-chlorosuccinimide and 1.46 g (0.0047 mole) of diphenyl diselenide. After 3 hours at room temperature the mixture was partitioned between 500 ml of hexane and 1000 ml of 5% Na2S2O3. The hexane was distilled off at atmospheric pressure and the residue was dissolved in 200 ml of DMF, 9.49 g (0.051 mole) of potassium phthalimide was added and the mixture was warmed to 90° C. under N2. After 45 min. the cooled reaction mixture was poured into water and the precipitated product was filtered off and recrystallized from ethylacetate/2-propanol, affording 3.57 g colorless crystals, mp. 136°-137° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04703058 |
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| 出典データセット | uspto-grants-1987_10 |
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| ORD ID | ord-7c326113c7934c3eaca585bb14d50dfc |
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| 出典メモ | uspto-grants-1987_10 |
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