関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylphosphine | HCID 27365 | — |
| 反応物 | 2,6-DI-Tert-butyl-4-thiocyanato-phenol | HCID 619245 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2,6-Di-tert-butyl-4-mercaptophenol | HCID 70370 | 86.9% |
反応手順
3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl thiocyanate (55 g, 0.209 mole) was dissolved in acetone (200 ml) under an argon atmosphere. Water (7.6 g, 0.42 mole) was added and the reaction cooled to 0° C. Triethylphosphine (24.7 g, 0.209 mole) was added dropwise over a period of 1 hour and the reaction was then allowed to warm to room temperature with stirring. The solution was concentrated, solvents removed, and the resulting oil purified by chromatography on silica. The fractions containing the thiol were combined, the solvents removed to yield a white powder which was recrystallized from methanol/water and dried to yield 43.3 g of the desired product. NMR confirmed the identity of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05162365 |
|---|
| 出典データセット | uspto-grants-1992_11 |
|---|
| ORD ID | ord-9e233d099bf94456ba97ffdf8ef13edd |
|---|
| 出典メモ | uspto-grants-1992_11 |
|---|