反应详情

温度

100 °C

To a suspension of crude sodium (2-bromophenyl)methanesulfonate (34 g) in toluene (500 mL) was added PCl5 (34 g, 0.16 mol). The resulting mixture was stirred at 100° Celsius for 4 hours before concentrating to dryness and pouring the residue onto crushed ice (150 g), stirring for 5 min, and extracting with DCM (3×50 mL). The combined organic extracts were dried over MgSO4, filtered and concentrated to dryness to give (2-bromophenyl)methanesulfonyl chloride (16.8 g, 77%). 1H NMR (300 MHz, DMSO-d6) δ 7.62-7.45 (m, 2H), 7.29 (m, 1H), 7.18-7.01 (m, 1H), 3.97 (s, 2H).

1. concentrationbefore concentrating to dryness
2. additionpouring the residue
3. customonto crushed ice (150 g)
4. stirringstirring for 5 min
5. extractionextracting with DCM (3×50 mL)
6. dry with materialThe combined organic extracts were dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated to dryness