関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3,5-Trithiane | HCID 9264 | — |
| 反応物 | 4'-Phenoxyacetophenone | HCID 236783 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-{1-(4-Phenoxyphenyl)-1-hydroxyethan-1-yl}-1,3,5-trithiane | HCID 14329268 | 70% |
反応手順
In 30 ml of anhydrous tetrahydrofuran was suspended 2.6 g of 1,3,5-trithiane, and 12 ml of 1.6M n-butyl lithium was added dropwise under an argon atmosphere at a temperature of about -20° C. After completion of the dropwise addition, the resulting mixture was stirred for 2 hours. Next, the reaction mixture was cooled to about -60° C., and then a solution of 4.0 g of 4-phenoxyacetophenone dissolved in 10 ml of tetrahydrofuran was dropped thereinto. After completion of the dropping, the reaction temperature was slowly raised to 0° C. The mixture thus obtained was stirred at 0° C. for another 1 hour. Thereafter, the same treatment as in Example 1 was carried out to obtain a crude product, which was then purified by a silica gel column chromatography (chloroform) to give 3.4 g of the desired compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05045562 |
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| 出典データセット | uspto-grants-1991_09 |
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| ORD ID | ord-16ba98998bca43b5b108e5d9646c706c |
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| 出典メモ | uspto-grants-1991_09 |
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