反应详情

Ethyl[(2,3-dimethylphenyl)oxy]acetate (6.1 g, 29.3 mmol) was added dropwise to chlorosulfonic acid (8.78 mL, 132 mmol) at 0° C., with stirring, causing a blood red solution. Reaction stirred for 30 minutes, then allowed to warm to RT. Mixture was stirred for a further 2 hours, then quenched by pouring over ice/water (200 mL). A dark red gum formed, this was extracted into dichloromethane (3×100 mL). Organics were concentrated in vacuo, to give a thick red oil, which crystallized on standing. Product was dried overnight in vacuum oven, to yield 8.179 g as red crystals. No further purification carried out. RT 1.25 mins.

1. customReaction
2. stirringstirred for 30 minutes
3. stirringMixture was stirred for a further 2 hours
4. customquenched
5. additionby pouring over ice/water (200 mL)
6. customA dark red gum formed
7. extractionthis was extracted into dichloromethane (3×100 mL)
8. concentrationOrganics were concentrated in vacuo
9. customto give a thick red oil, which
10. customcrystallized
11. customProduct was dried overnight in vacuum oven
12. customto yield 8.179 g as red crystals
13. customNo further purification
14. customRT 1.25 mins