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Sodium Hydroxide → 2,6-Di-sec-butylphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Carbamic acid 2,6-di-sec-butylphenyl ester | HCID 66725334 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 2,6-Di-sec-butylphenol | HCID 21685 | 100.3% |
反応手順
R-(+)-1-Phenyl-ethyl)-carbamic acid (−)-2,6-di-sec-butylphenyl ester (1b) (4.1 g, 11.6 mmol) was dissolved in a 100 ml 1:1 mixture of dioxane: 1M NaOH aq. The reaction mixture was stirred at 70° C. for 15 min. Volatiles were removed at reduced pressure to a volume of ˜50-70 ml. The pH was adjusted to 3-4 with 1M HCl. The phenol was extracted with ether (3×50 ml), washed with 1 M HCl, brine and dried over anhydrous MgSO4. Evaporation yielded crude yellow oil (2.4 g, ˜100%). Vacuum distillation was performed (120-125° C./˜5 mm) (2.1 g, 89%). Optical rotation: α20D=−14.11° (c=2, pentane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08071818B2 |
| 出典データセット | uspto-grants-2011_12 |
| ORD ID | ord-f1cd41664aa64e849f57788cd4e41764 |
| 出典メモ | uspto-grants-2011_12 |