化工社化工社 化学情報印刷レポート · 研究参考用
Tributylstannane → 4-Benzoyloxy-1-t-butoxy-2,2,6,6-tetramethylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | 2-Iodo-2-methylpropane | HCID 11206 | — |
| 反応物 | 1-Hydroxy-4-benzoyloxy-2,2,6,6-tetramethylpiperidine | HCID 688178 | — |
| 溶媒 | Chlorobenzene | HCID 7964 | — |
| 生成物 | 4-Benzoyloxy-1-t-butoxy-2,2,6,6-tetramethylpiperidine | HCID 12996907 | 44.5% |
反応手順
A solution of 56.0 g (203 mmol) of 4-benzoyloxy-1-oxyl-2,2,6,6-tetramethylpiperidine, 125 ml of chlorobenzene, and 58.9 g of t-butyl iodide is cooled to 5° C. Tri-n-butyltin hydride (29 g, 100 mmol) is added dropwise over 110 minutes while the temperature is maintained below 20° C. The reaction mixture is concentrated at reduced pressure and then purified by silica gel chromatography (200:1, then 100:3 heptane:ethyl acetate) to afford 30.1 g of a white solid, m.p. 80°-82.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05204473 |
| 出典データセット | uspto-grants-1993_04 |
| ORD ID | ord-03b8a0f652b34942ad38273eb81f18a7 |
| 出典メモ | uspto-grants-1993_04 |