反应详情

温度

0 °C

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.

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 which
8. customwas recrystallized from methanol/water
9. customdried