反应详情

温度

65 °C

Mix 3-(4-nitrophenoxy)propanoic acid (6.5 g, 30 mmol) and concentrated H2SO4 (30 mL). Once dissolved, add P2O5, stir at 65° C. for 3 hrs. Cool to room temperature, pour slowly the reaction mixture to ice water (50 mL), stir for 15 min, and extract with EtOAc (100 mL×3). Combine the organic layers, wash with brine (100 mL×2), dry over anhydrous Na2SO4, concentrate to give the crude product. Purification by chromatography (silica gel, EtOAc:PE=1:1) affords the title compound (4.6 g, 77.8%). MS: (M−1): 192.2.

1. dissolutionOnce dissolved
2. temperatureCool to room temperature
3. stirringstir for 15 min
4. extractionextract with EtOAc (100 mL×3)
5. washCombine the organic layers, wash with brine (100 mL×2)
6. dry with materialdry over anhydrous Na2SO4
7. concentrationconcentrate
8. customto give the crude product
9. customPurification by chromatography (silica gel, EtOAc:PE=1:1)