化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2-Nitrobenzyl perfluorooctanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Triethylamine hydrochloride | HCID 11130 | — |
| 反応物 | 2-Nitrobenzyl alcohol | HCID 11923 | — |
| 反応物 | Perfluorooctanoyl chloride | HCID 78978 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-Nitrobenzyl perfluorooctanoate | HCID 15095406 | — |
反応手順
Perfluorooctanoyl chloride (21.6 g, 0.05 mol) was added slowly with stirring to a solution of 2-nitrobenzyl alcohol (7.65 g, 0.05 mol) and triethylamine (5.2 g, 0.05 mol) in 100 ml benzene. During the addition, the temperature was allowed to rise to 50° C. and the triethylamine hydrochloride began to precipitate. After the addition was complete, the reaction was stirred an additional 30 minutes. The reaction was filtered and the filtrate evaporated in vacuo to give an oil which crystallized on cooling in an ice bath (m.p. 34°-35° C.). Benzene washings of the material retained on the filter paper gave a second fraction of oil which crystallized on cooling. Total yield was 11.97 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04980096 |
| 出典データセット | uspto-grants-1990_12 |
| ORD ID | ord-90dad4268b454d1e82866a9156e0c4f0 |
| 出典メモ | uspto-grants-1990_12 |