反应详情

温度

0 °C

To a cooled solution of 5-(2,6-dichloro-4-nitro-phenoxy)-2-methoxy-benzenesulfonyl chloride (920 mg, 2.2 mmol) in CH2Cl2 (25 mL) at 0° C. was added triethylamine (470 μL, 3.4 mmol) and cyclopropylamine (170 μL, 2.5 mol). The resulting mixture was stirred at 0° C. for 5 min, then at RT for 6 h. Water (30 mL) and 1N HCl (1 mL) was added and the solution was extracted with EtOAc (3×50 mL). The combined EtOAc extracts were dried and concentrated. The product was purified by chromatography to give the title compound of Step B (652 mg). MS (APCl) Calc.: 432.0. Found: 430.9 (M−1).

1. waitat RT for 6 h
2. extractionthe solution was extracted with EtOAc (3×50 mL)
3. dry with materialThe combined EtOAc extracts were dried
4. concentrationconcentrated
5. customThe product was purified by chromatography