関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Xanthene | HCID 7107 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | 1-(9H-xanthen-2-yl)ethanone | HCID 515178 | — |
反応手順
A 21.4 ml portion of acetyl chloride in 30 ml of 1,2-dichloroethane was added dropwise to 40 g of aluminum chloride in 105 ml of 1,2-dichloroethane. This mixture was stirred 1/2 hour and then added portionwise to an ice-cooled solution of 54.66 g of xanthene in 225 ml of 1,2-dichloroethane. The reaction was then allowed to warm to 16° C. and poured onto ice. A 180 ml portion of concentrated hydrochloric acid was added, the mixture was allowed to stand overnight and the layers separated. The aqueous layer was extracted with two 100 ml portions of chloroform then the organic layers was combined, dried, filtered through hydrous magnesium silicate and evaporated, giving the desired intermediate as a white crystalline solid, mp 103°-104° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04613611 |
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| 出典データセット | uspto-grants-1986_09 |
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| ORD ID | ord-34713538c47747c8aa1843aa62c6c141 |
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| 出典メモ | uspto-grants-1986_09 |
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