反应详情

To a solution of ethyl 2-chloroacetate (0.5 g, 5.74 mmol) in DMF (70 ml) at 10° C. were added K2CO3 (1.98 g, 14.34 mmol, 2.5 eq.) and 1-methylpiperazine (1.05 g, 8.6 mmol, 1.5 eq.) and the mixture was stirred at RT for 2 h. The mixture was quenched and extracted as in Intermediate Example 5(c). The solvent was distilled off and the crude residue was purified by column chromatography (60-120 silica gel, 40% ethyl acetate in hexane) to afford the product in 74% yield (0.74 g). LC-MS (ESI): Calculated mass: 173.2, Observed mass: 174.0 [M+H]+ (rt: 0.20 min).

1. customThe mixture was quenched
2. extractionextracted as in Intermediate Example 5(c)
3. distillationThe solvent was distilled off
4. customthe crude residue was purified by column chromatography (60-120 silica gel, 40% ethyl acetate in hexane)
5. customto afford the product in 74% yield (0.74 g)
6. custom174.0 [M+H]+ (rt: 0.20 min)