反应详情

To a solution of 2-chloro-N-(2,4-dihydroxyphenyl)acetamide (20 g, 0.0995 mol) in CH2Cl2 (250 mL) sodium hydride (7.164 g, 0.2985 mol) was slowly added at RT. The resulting mixture was stirred for 6 h before water (10 mL) was slowly added. The solution was concentrated in vacuo and purified with column chromatography using 100% CH2Cl2→25%→40% 90:10:1 CH2Cl2:MeOH:NH4OH to yield the title compound. MS (ESI, pos. ion) m/z: 166 (M+1). Mass cal'd for C8H7NO3: 165.04.

1. additionwas slowly added
2. concentrationThe solution was concentrated in vacuo
3. custompurified with column chromatography