化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → alpha-(o-Fluorobenzoylthiomethyl)-beta-phenyl-gamma-butyrolactone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Fluorobenzoic acid | HCID 9935 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | alpha-Mercaptomethyl-beta-phenyl-gamma-butyrolactone | HCID 13518975 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | alpha-(o-Fluorobenzoylthiomethyl)-beta-phenyl-gamma-butyrolactone | HCID 13518918 | 67.2% |
反応手順
To a solution of 1.2 g of o-fluorobenzoic acid and 1.5 g of α-mercaptomethyl-β-phenyl-γ-butyrolactone in 20 ml of dimethylformamide were added 1.9 ml of diphenylphosphoryl azide (DPPA) and then 1.2 ml of triethylamine under ice-cooling. Then, the mixture was raised to a room temperature and stirred for 18 hours. After completion of the reaciton, the reaction mixture was diluted with 200 ml of ethyl ether, washed with 5% hydrochloric acid, saturated aqueous sodium hydrogencarbonate, and saturated saline, dried over magnesium sulfate and the solvent was then distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 1.6 g (yield 67%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04613613 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-0a89f202a1ce4947b408e89c52abab67 |
| 出典メモ | uspto-grants-1986_09 |