反应详情

2-Nitro-5-fluorophenol (3.0 g) and tert-butyl-N-(2-hydroxypropyl)carbamate were dissolved in THF (20 ml) and triphenylphosphine (7.5 g) and di-tert-butyl-azodicarboxylate were added. The exothermic reaction was cooled in an ice bath. Then the reaction mixture was stirred at room temperature for 2 h. The mixture was concentrated in vacuo and the residue was purified by chromatography (silica gel/dichloromethane: petroleum ether 1:2). The fractions were combined and concentrated in vacuo. The residue was dissolved in dichloromethane and washed with 1M NaOH. The organic layer was separated, dried, filtered and concentrated in vacuo.

1. customThe exothermic reaction
2. temperaturewas cooled in an ice bath
3. concentrationThe mixture was concentrated in vacuo
4. customthe residue was purified by chromatography (silica gel/dichloromethane: petroleum ether 1:2)
5. concentrationconcentrated in vacuo
6. dissolutionThe residue was dissolved in dichloromethane
7. washwashed with 1M NaOH
8. customThe organic layer was separated
9. customdried
10. filtrationfiltered
11. concentrationconcentrated in vacuo