反应详情

温度

-50 °C

To a solution of 2,4-dihydroxy benzoic acid (3.08 g; 20 mmol) in dioxane (50 mL) was added conc. H2SO4 (3 mL) and the solution was cooled to −50° C. Isobutene (40 g) was added, the reaction flask sealed and allowed to warm to room temperature. The reaction mixture was stirred overnight, cooled to −30° C. and pH adjusted to 8 using saturated NaHCO3 (aq). The organic phase was Isolated, dried, evaporated to dryness and purified by column chromatography (SiO2-heptane/EtOAc=4:1) to yield 2.3 g (54%). MS (LC-MS): 209 (MH−).

1. customthe reaction flask sealed
2. temperatureto warm to room temperature
3. temperaturecooled to −30° C.
4. customThe organic phase was Isolated
5. customdried
6. customevaporated to dryness
7. custompurified by column chromatography (SiO2-heptane/EtOAc=4:1)
8. customto yield 2.3 g (54%)