化工社化工社 化学情報印刷レポート · 研究参考用
Ammonia → Tetradec-7-yn-1,14-dial dimethylacetal
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Lithium amide | HCID 24532 | — |
| 反応物 | Lithium | HCID 3028194 | — |
| 反応物 | 1,1-Dimethoxy-6-iodohexane | HCID 20526840 | — |
| 反応物 | 1,1-Dimethoxy-oct-7-yne | HCID 20526849 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Tetradec-7-yn-1,14-dial dimethylacetal | HCID 20526841 | 84.5% |
反応手順
To a stirred suspension of lithium amide, prepared from 1.45 g (0.21 atom) of lithium in ca. 200 ml of liquid ammonia was added 30.6 g (0.18 Mole) of 1,1-dimethoxy-oct-7-yne over a period of 10 min. Dimethyl-sulfoxide (100 ml) was then added, followed by 62.5 g (0.23 Mole) of 1,1-dimethoxy-6-iodohexane within 10 min. Work-up as above gave an oil, from which low-boiling impurities were removed by heating at 100°/0.05 Torr. Crude tetradec-7-yn-1,14-dial dimethylacetal (40.8 g, 72% yield) was used without further purification. A sample was submitted to a rapid distillation: b.p. 140°/0.05 Torr.--IR: 1125, 1070, 1050 cm-1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04346023 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-87f56a3cfd314d67914e508a925488f4 |
| 出典メモ | uspto-grants-1982_08 |