反应详情

温度

120 °C

A mixture of 68 (8.2 g, 0.028 mol), phosphorous tribromide (80 mL) and N,N-dimethylaniline (5 mL) was heated to 120° C. for 3 h. After cooling, the reaction mixture was carefully poured into ice, extracted with EtOAc, and purified by silica gel column chromatography, providing 69(2.5 g) as a yellow solid. MS: 349.1, 351.1 (M+1). 1HNMR (DMSO-d6) ppm 8.82 (s, 1H), 7.55-7.41 (m, 10H).

1. temperatureAfter cooling
2. additionthe reaction mixture was carefully poured into ice
3. extractionextracted with EtOAc
4. custompurified by silica gel column chromatography