関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | gamma-Propanol | HCID 169766 | — |
| 溶媒 | Trifluoroacetic acid | HCID 6422 | — |
| 生成物 | 4-(3-Hyd-roxypropyl)-2-t-butylphenol | HCID 13405065 | 76.2% |
反応手順
A stirred solution of III (12.5 Kg) in trifluoroacetic acid (60.0 L) was heated 40° C. for 6 hrs. After completion of reaction on TLC, reaction mixture was quenched in ice-water and extracted 3 times with dichloromethane (25.0 L). Total organic layers were combined and evaporated to dryness at atmospheric pressure. A solution of sodium hydroxide (3.0 Kg) in methanol (50.0 L) was added to the residue and stirred at room temperature for 1 hr. The solution was neutralized with 1N HCl and extracted 3 times with dichloromethane (25.0 L). All the organic layers were combined and washed with saturated sodium carbonate solution (10.0 L), DM Water (10.0 L), brine (10.0 L) and evaporated to dryness under reduced pressure to give the title compound (7.5 Kg)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07825257B1 |
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| 出典データセット | uspto-grants-2010_11 |
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| ORD ID | ord-ebba5e16d5fc49b6b9e9838f05b3786e |
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| 出典メモ | uspto-grants-2010_11 |
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