関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | o-Phenetidine | HCID 7203 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | o-Methylbenzoyl bromide | HCID 2753161 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | N-(2-Ethoxyphenyl)-2-methylbenzamide | HCID 576828 | 94.5% |
反応手順
A 19.9 g (0.1 mol) portion of o-methylbenzoyl bromide was added dropwise with cooling to a mixture of 13.7 g (0.1 mol) of o-ethoxyaniline and 8.4 g (0.1 mol) of sodium bicarbonate in 200 ml of acetone with stirring. After addition of the o-methylbenzoyl bromide, the reaction mixture was warmed to 40° C and the mixture was refluxed and stirred for another 40 hours. After filtering, the ether was distilled from the reaction mixture and the residual material was re-dissolved in ether and washed with water. The ether layer was dried over anhydrous sodium sulfate, the ether was removed and the product was distilled to obtain 24.1 g (94.5%) of a clear pink liquid having a boiling point of 148° C/0.04 mm Hg and nD20 of 1.5929.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03985804 |
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| 出典データセット | uspto-grants-1976_10 |
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| ORD ID | ord-f753bb8743d34f2faa04ac641cf2bb14 |
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| 出典メモ | uspto-grants-1976_10 |
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