化工社化工社 化学情報印刷レポート · 研究参考用
Bromide ion → 1-(3,5-Di-tert-butyl-4-hydroxyphenyl)-2-[(pyridin-2-ylmethyl)amino]ethanone hydrobromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromide ion | HCID 259 | — |
| 反応物 | 2-Pyridinemethanamine | HCID 19509 | — |
| 反応物 | 2-Bromo-1-[3,5-di(tert-butyl)-4-hydroxyphenyl]ethan-1-one | HCID 616161 | — |
| 反応物 | Lithium bis(trimethylsilyl)amide | HCID 57426343 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(3,5-Di-tert-butyl-4-hydroxyphenyl)-2-[(pyridin-2-ylmethyl)amino]ethanone hydrobromide | HCID 86632958 | 48.8% |
反応手順
2-(Aminomethyl)pyridine (100 mg) was initially introduced in absolute THF (12 ml) and treated with lithium hexamethyldisilazane solution (1.01 ml, 1 M in THF) at RT with stirring and under argon. After 30 min, 2-bromo-1-(3,5-di-tert-butyl-4-hydroxyphenyl)ethanone (0.5 eq., 151 mg, dissolved in 1.5 ml absolute THF) was added dropwise. For completion of the reaction, the remaining amount of bromide (151 mg) was added and after 2 hours the precipitate formed was filtered off with suction and dried. The 98 mg of the title compound obtained are contaminated with small amounts of THF which, however, do not interfere with the further reaction.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863269B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-95d0713d57cf489f97dd908458377bb5 |
| 出典メモ | uspto-grants-2011_01 |