関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Salicylate | HCID 8365 | — |
| 反応物 | Tetrabutylammonium Hydroxide | HCID 2723671 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178449046 | HCID 178449046 | — |
反応手順
A glass flask with reflux condenser, heatable oil bath, mechanical stirrer and internal thermometer was charged at room temperature with 35.90 g of ethyl salicylate and 282.13 g of water and these components were stirred together thoroughly. Subsequently 139.98 g of tetrabutylammonium hydroxide (40% strength in water) were added and the reaction mixture was heated to 60° C. It was stirred at 60° C. for one hour (the contents of the flask become clear). Then the reaction mixture was cooled and the water was distilled off under reduced pressure, 20 mbar, at 30-45° C. The residue was taken up at 60° C. in 200 ml of toluene. Subsequently the mixture was redistilled. The residue was recrystallized from 50 ml of butyl acetate. The product was filtered off, washed with butyl acetate and dried at 80° C. and 10 mbar in a vacuum drying cabinet. This gave a white solid having a melting point of 93° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07381785B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-9b461631879345bd92daf1ca4edaa640 |
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| 出典メモ | uspto-grants-2008_06 |
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