反应详情

温度

100 °C

A mixture of methyl 4-hydroxy-3-nitrobenzoate (1.00 g, 5.07 mmol) and concentrated aq ammonia (10.0 mL, 162 mmol) was heated to 100° C. for 90 mins (3×30 mins) in a microwave reactor. The mixture was poured into water (70 mL), acidified with 6N HCl and extracted with EtOAc (4×25 mL). The combined extracts were dried (MgSO4) and concentrated in vacuo. The residue was triturated with DCM (20 mL) filtered and washed with DCM before drying under vacuum to afford the crude title compound as a yellow solid 0.49 g, 53.0%

1. extractionextracted with EtOAc (4×25 mL)
2. dry with materialThe combined extracts were dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customThe residue was triturated with DCM (20 mL)
5. filtrationfiltered
6. washwashed with DCM
7. custombefore drying under vacuum