化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → 3-(3,5-Di-tert-butyl-4-hydroxyphenyl)-1-methyl-pyrrolidine-2,5-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,6-Di-tert-butylphenol | HCID 31405 | — |
| 反応物 | N-Methylmaleimide | HCID 70261 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 3-(3,5-Di-tert-butyl-4-hydroxyphenyl)-1-methyl-pyrrolidine-2,5-dione | HCID 14148374 | 9.5% |
反応手順
This compound is prepared by the procedure of Example 1 from 2.40 g (0.1 mol) of sodium hydride, 20.63 g (0.1 mol) of 2,6-di-tert-butylphenol, and 11.11 g (0.1 mol) of N-methylmaleimide in tert-butyl alcohol. The residue is recrystallized from petroleum ether to give 13.2 g (42%) of crude product. The analytical sample is prepared by flash chromatography (1:1 heptane:ethyl acetate eluent) followed by trituration with a mixture of heptane and toluene to give 3.0 g of a white solid: mp 164°-166° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04709050 |
| 出典データセット | uspto-grants-1987_11 |
| ORD ID | ord-53eea7b7a4c14ee1888689b3797f1755 |
| 出典メモ | uspto-grants-1987_11 |