化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Tert-butyl 3-(4-{[(1-adamantylmethyl)amino]-carbonyl}-5-chloropyridin-2-yl)prop-2-ynyl(ethyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | tert-butyl N-ethyl-N-(prop-2-yn-1-yl)carbamate | HCID 18366151 | — |
| 反応物 | N-(1-adamantylmethyl)-5-chloro-2-iodoisonicotinamide | HCID 21906675 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Tert-butyl 3-(4-{[(1-adamantylmethyl)amino]-carbonyl}-5-chloropyridin-2-yl)prop-2-ynyl(ethyl)carbamate | HCID 21906729 | 66.5% |
反応手順
The sub-titled compound was prepared from N-(1 adamantylmethyl)-5-chloro-2-iodoisonicotinamide (Example 2(i)) (0.40 g), tert-butyl ethyl(prop-2-ynyl)carbamate (Example 7(i)) (0.34 g), copper (I) iodide (0.004 g), bis-triphenyphosphine palladium dichloride (0.014 g), triethylamine (5 ml) and anhydrous acetonitrile (5 ml) by the method of Example 2(iii). The crude product was purified by chromatography on silica gel eluting with iso-hexane:ethyl acetate (9:1 to 7:3) to afford the sub-titled compound (0.30 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129246B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-6d8ec4b762d2485e9095644448ce1180 |
| 出典メモ | uspto-grants-2006_10 |