反应详情

温度

0 °C

3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenylthiocyanate (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 and the solvents removed to yield a white powder. Recrystallization from methanol/water yielded, upon drying, 43.3 g of the title compound. The NMR spectrum confirmed the identity of the product.

1. temperatureto warm to room temperature
2. concentrationThe solution was concentrated
3. customsolvents removed
4. customthe resulting oil purified by chromatography on silica
5. additionThe fractions containing the thiol
6. customthe solvents removed
7. customto yield a white powder
8. customRecrystallization from methanol/water
9. customyielded
10. customupon drying