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Potassium Hydroxide → 5-(1-Adamantylethynyl)isophthalic acid dipotassium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1-(3,5-Bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne | HCID 67507300 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 5-(1-Adamantylethynyl)isophthalic acid dipotassium salt | HCID 67506617 | 97% |
反応手順
In a 5 L four-neck flask provided with a thermometer, a Dimroth condenser and an agitator, 3 L of n-butanol and 226 g of potassium hydroxide (85%) (2.72 mol) were charged. The mixture was heated and refluxed to be dissolved. After adding 120 g of the obtained 1-(3,5-bis(methoxycarbonyl)phenyl)-2-(1-adamantyl)ethyne (0.341 mol) therein, the mixture was heated and refluxed for 30 minutes. Next, it was cooled in an ice bath and filtered to obtain precipitated crystal. The crystal was washed with 1 L of ethanol two times followed by drying under pressure at 60° C., thus obtaining 132.49 g of 5-(2-(1-adamantyl)ethynyl) isophthalic acid dipotassium salt (the yield was 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07652125B2 |
| 出典データセット | uspto-grants-2010_01 |
| ORD ID | ord-13a4d2f0e7544239ab7abc05a4ff91b6 |
| 出典メモ | uspto-grants-2010_01 |