関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (Chloromethyl)cyclopropane | HCID 80013 | — |
| 反応物 | 1-Acetamido-7-naphthol | HCID 80946 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | N-[7-(Cyclopropylmethoxy)naphth-1-yl]acetamide | HCID 22400263 | 59.9% |
反応手順
17.1 g (0.085 mol) of N-(7-hydroxynaphth-1-yl)acetamide in solution in 50 ml of dimethyl sulphoxide are added under a nitrogen atmosphere to a suspension of 3.4 g (0.085 mol) of sodium hydride in oil, washed beforehand with dry pentane), in 100 ml of dimethyl sulphoxide, while the mixture is cooled with an ice-water bath. Stirring is continued at room temperature for 2 h. 9.05 g (0.1 mol) of (chloromethyl)cyclopropane are added, and the mixture is stirred at room temperature for 4 h and left to stand overnight. The mixture is poured into 1 l of water, stirred for 1 h and left to stand overnight under cold conditions. The solid is separated by filtration, washed with water and dried. 13 g of a product melting point: 154°-155° C., are obtained which is used as it is in the following step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05530002 |
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| 出典データセット | uspto-grants-1996_06 |
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| ORD ID | ord-f7008c6b03ac4d55ada0fd490ad51b40 |
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| 出典メモ | uspto-grants-1996_06 |
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