反应详情

温度

80 °C

A flask was charged with 491 mg (2.12 mmol) of solid 2-(4-nitro-phenyl)-ethanesulfonic acid (as prepared in the previous step), which was treated with 3.10 mL (42.4 mmol) of thionyl chloride and heated to 80° C. for 7 h. The volatile components were removed in vacuo, the residue was taken up in THF (20 mL), and 927 μL (10.6 mmol) of morpholine was added. The mixture was stirred at RT for 16 h, diluted with water (15 mL) and saturated aqueous NaHCO3 (15 mL) and extracted with EtOAc (2×70 mL). The organic layer was dried (MgSO4) and concentrated in vacuo to afford 370 mg (52%) of the title compound as a pale yellow solid: 1H-NMR (CDCl3; 400 MHz): δ 8.20 (d, 2H, J=8.8 Hz), 7.40 (d, 2H, J=8.8 Hz), 3.79-3.73 (m, 4H), 3.31-3.23 (m, 6H), 3.21-3.14 (m, 2H).

1. customas prepared in the previous step), which
2. customThe volatile components were removed in vacuo
3. extractionextracted with EtOAc (2×70 mL)
4. dry with materialThe organic layer was dried (MgSO4)
5. concentrationconcentrated in vacuo