反应详情

2-(4-t-butylphenyl)-3-hydroxy-4-methylcarbonylthiophene (2.66 g, 9.7 mmol), N-bromosuccinimide (1.73 g, 9.7 mmol) and benzoyl peroxide (153 mg, 0.63 mmol) were heated with reflux for 2 hours in 65 ml of chloroform. Water was added, and the reaction solution was extracted three times with chloroform, and the organic layer was washed with a saturated aqueous sodium chloride solution, and then dried over anhydrous sodium sulfate. The obtained organic layer was concentrated, and then purified with a silica gel column chromatography (n-hexane/chloroform=3/2) to obtain the desired product as a yellow solid (2.93 g, yield 86%).

1. extractionthe reaction solution was extracted three times with chloroform
2. washthe organic layer was washed with a saturated aqueous sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. concentrationThe obtained organic layer was concentrated
5. custompurified with a silica gel column chromatography (n-hexane/chloroform=3/2)