反应详情

温度

0 °C

To a solution of (2-amino-4,5-dimethoxyphenyl)(3-bromophenyl)methanone (5 g, 14.9 mmol) in dry DCM (125 mL) was added thiophen-2-ylacetic acid (2.54 g, 17.9 mmol) and Et3N (6.77, 66.9 mmol) at 0° C. in N2. 10 minutes later, POCK (3.4 g, 22.31 mmol) was added dropwise at 0° C. in N2. The reaction mixture was stirred for 1 hour at 0° C. and then quenched with saturated NaHCO3, and neutralized to pH=8. The mixture was exacted with ACM (30 mL×3). The combined organic layer was dried over anhydrous MgSO4, filtered and concentrated under vacuum to afford N-{2-[(3-bromophenyl)carbonyl]-4,5-dimethoxyphenyl}-2-(thiophen-2-yl)acetamide. MS (M+H)=460 and 462.

1. customquenched with saturated NaHCO3
2. dry with materialThe combined organic layer was dried over anhydrous MgSO4
3. filtrationfiltered
4. concentrationconcentrated under vacuum