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Methanol → HCID 15782683、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Nitrotricyclo(3.3.1.13,7)decane-1-carboxylic acid | HCID 39239 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 15782683 | HCID 15782683 | 95% |
反応手順
In an atmosphere of nitrogen, 10 mmole of 1-carboxy-3-nitroadamantane obtained by the method of Example 42 was dissolved in 10ml of DMF. To the mixture, 15 mmole of acetyl chloride was added dropwise over 30 minutes. The mixture was heated to begin to reflux around the conclusion of the addition. After refluxing for 2 hours, the mixture was cooled, 20 mmole of triethylamine was added, and then 11 mmole of methanol was added dropwise over 30 minutes while retaining the temperature of the mixture at 10° C. or less followed by stirring for more 2 hours. As a result, the conversion of 1-carboxy-3-nitroadamantane was 99%, and 1-methoxycarbonyl-3-nitroadamantane (yield 95%) was formed.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06468487B1 |
| 出典データセット | uspto-grants-2002_10 |
| ORD ID | ord-2797b2fbc30c4e2f9176f399c466e35e |
| 出典メモ | uspto-grants-2002_10 |