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Lithium amide → 2,6-Diethyl-2,3,6-trimethyl-4-piperidyl p-t-butylbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium amide | HCID 24532 | — |
| 反応物 | Methyl p-tert-butylbenzoate | HCID 97433 | — |
| 反応物 | 2,6-Diethyl-2,3,6-trimethylpiperidin-4-ol | HCID 22182241 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 2,6-Diethyl-2,3,6-trimethyl-4-piperidyl p-t-butylbenzoate | HCID 21330294 | 104.2% |
反応手順
15.0 g of 2,6-diethyl-2,3,6-trimethyl-4-piperidinol (Compound 1) and 16.0 g of methyl p-t-butylbenzoate were dissolved in 500 ml of heptane. 1.5 g of lithium amide were then added to the solution and the mixture was refluxed by heating in a flask equipped with a Dean-Stark separator. 1.5 g of methanol were first removed and this was followed by 200 ml of heptane, which distilled off over a period of 3 hours. After cooling the reaction mixture, it was washed with water and dried over magnesium sulphate; the solvent was then removed by evaporation under reduced pressure. The residue was distilled under reduced pressure, giving 28.2 g of the title compound as a colourless liquid (bp 176° - 178° C/0.008 mmHg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04075165 |
| 出典データセット | uspto-grants-1978_02 |
| ORD ID | ord-d370690fe33242139b3c91d1546af39b |
| 出典メモ | uspto-grants-1978_02 |