反应详情

温度

60 °C

To a solution of 11 (74.0 g, 260 mmol) in toluene (370 mL) was added thionyl chloride (95 mL, 1300 mmol) in DMF (2.5 mL, 26 mmol) and the mixture was heated to reflux for 4 h. The mixture was cooled to approximately 60° C. and filtered to remove insoluble material. The filtrate was concentrated under reduced pressure and residual thionyl chloride was co-evaporated with toluene (2×120 mL) to give crude 12 which was used without purification.

1. temperaturethe mixture was heated
2. temperatureto reflux for 4 h
3. filtrationfiltered
4. customto remove insoluble material
5. concentrationThe filtrate was concentrated under reduced pressure and residual thionyl chloride
6. customto give crude 12 which
7. customwas used without purification