反应详情

温度

50 °C

To a solution of (4-methyl-thiazol-2-yl)-methanol (7.0 g, 54.3 mmol) in DMF (80 mL) was added NBS (10.6 mg, 59.6 mmol), and the mixture was stirred at 50° C. overnight. TLC (petroleum ether:EtOAc 2:1) indicated the reaction was completed. The mixture was diluted with H2O (50 mL) and extracted with EtOAc (50 mL×3). The combined organic layers were washed with brine (50 mL×3), dried over sodium sulfate, and concentrated in vacuum to give the residue which was purified by a silica gel column (petroleum ether:EtOAc 10:1) to give the title compound (11.2 g, 99%) as a brown solid.

1. extractionextracted with EtOAc (50 mL×3)
2. washThe combined organic layers were washed with brine (50 mL×3)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuum
5. customto give the residue which
6. customwas purified by a silica gel column (petroleum ether:EtOAc 10:1)