関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Benzoyl chloride | HCID 7412 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 2,5-Hexanediol | HCID 18049 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,5-Hexanediol dibenzoate | HCID 5259446 | 94% |
反応手順
To 2.4 g (0.02 mol) 2,5-hexanediol was added 30 ml tetrahydrofuran, then added 4.8 ml (0.06 mol) pyridine with stirring. To the resulting homogenous mixture was slowly added 5.8 ml (0.05 mol) benzoyl chloride, and the reaction was stirred at room temperature for 1 hour, then heated refluxing for 5 hours. Upon completing the reaction, 20 ml water was added to dissolve the resulting salt. The mixture was extracted with ethyl acetate. The organic phase was separated, washed with saturated saline for two times, and dried over anhydrous sodium sulfate. The solvent was removed. Distillation under reduced pressure gave colorless liquid 2,5-hexanediol dibenzoate, and the yield was 94%. 1HNMR: δ (ppm) 1.36(d, 6H, CH3), 1.86(m, 4H, CH2), 5.21(m, 2H, CH), 7.40-8.16(m, 10H, ArH)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07388061B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-c7485da0c3a449b786a71169a14152f2 |
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| 出典メモ | uspto-grants-2008_06 |
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