関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Peracetic Acid | HCID 6585 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Cinnamyl Alcohol | HCID 5315892 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-Phenyloxiranyl)methanol | HCID 89553 | — |
反応手順
Sodium carbonate (224 g) and trans-cinnamyl alcohol (200.0 g) were mixed with 2 L of methylene chloride, a slow nitrogen sweep was maintained through the vapor space of the flask and the mixture was cooled to 15-20° C. with a cold water bath. Peracetic acid solution (35%, 381.2 mL) was added over a 3 hour period, maintaining the internal temperature below 25° C. After the peracetic acid addition was complete, the mixture was stirred for 2-3 hours until complete, as shown by HPLC analysis. The mixture was cooled to 10° C. with an ice bath, and a solution of sodium sulfite (160 g) in 1200 ml water was added slowly over 90 minutes, keeping the temperature below 30° C. The phases were separated and the aqueous phase was extracted with methylene chloride (200 mL) to give a solution of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06376711B1 |
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| 出典データセット | uspto-grants-2002_04 |
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| ORD ID | ord-9efba723aa8449eabeb4caeeebe8fd59 |
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| 出典メモ | uspto-grants-2002_04 |
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