反应详情

To a stirred solution of 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 4, 0.2 g, 0.64 mmol) and 2-(p-tolyloxy)acetic acid (106 mg, 0.64 mmol) in dry DCM (20 mL), DIPEA (495 mg, 3.86 mmol) followed by HATU (486 mg, 1.27 mmol) was added at room temperature and stirred overnight. The mixture was then diluted with DCM and washed with water (2×10 mL) & brine (2×10 mL). The organic extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by column chromatography to yield the title compound (0.21 g, 77.5%) as an off-white solid.

1. additionwas added at room temperature
2. washwashed with water (2×10 mL) & brine (2×10 mL)
3. extractionThe organic extract
4. dry with materialwas dried over anhydrous sodium sulphate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified by column chromatography