反应详情

A solution of 4-chloro-3-nitrobenzoyl chloride (1.336 g, 6.681 mmol) in anhydrous pyridine (30 mL) was treated with 2-amino-5-tert-butylthiazole (1.044 g, 6.681 mmol) and the reaction stirred at room temperature under a nitrogen atmosphere. The solvent was removed by rotary evaporation in vacuo and the residue dried on a vacuum pump. The residue was taken up in ethyl acetate (100 mL) and washed with water (4×50 mL) and brine (50 mL). The organic phase was dried over anhydrous sodium sulfate, filtered, and concentrated in vacuo. Purification by silica gel chromatography eluting with 5% ethyl acetate/methylene chloride provided the title compound (1.76 g, 78%).

1. customThe solvent was removed by rotary evaporation in vacuo
2. customthe residue dried on a vacuum pump
3. washwashed with water (4×50 mL) and brine (50 mL)
4. dry with materialThe organic phase was dried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification by silica gel chromatography
8. washeluting with 5% ethyl acetate/methylene chloride