関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2,3-Dimethylacrylic acid, (Z)- | HCID 643915 | — |
| 反応物 | 2,4,6-Trichlorobenzoyl chloride | HCID 2733703 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 10924839 | HCID 10924839 | 33% |
反応手順
Angelic acid (601 mg, 6.0 mmol) was dissolved in dichloromethane (3.0 mL) under argon. Diisopropylethylamine (1.23 mL, 7.20 mmol) was added at 5-10° C. in a period of 1 min. To this solution was added 2,4,6-trichlorobenzoyl chloride (1.12 mL, 7.20 mmol) at 3-6° C. in a period of 4 min. After the reaction solution had been stirred at 2° C. for 45 min, petroleum ether (9.0 mL) was added. The obtained suspension was purified by flash chromatography (petroleum ether/dichloromethane 3:1), giving the title compound as a white solid (605 mg, 33%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08901356B2 |
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| 出典データセット | uspto-grants-2014_12 |
|---|
| ORD ID | ord-d664243ed8d84e8ca51746c237f6fc43 |
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| 出典メモ | uspto-grants-2014_12 |
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