反应详情

温度

50 °C

Trimethylsilylchloride (9.1 mL) was added to a stirred solution of 3-iodobenzaldehyde (15.1 g) and formamide (6.5 mL) in MeCN (34 mL) and toluene (34 mL) under an inert atmosphere. The reaction was then heated at 50° C. for 5 hours. Toluene sulfinic acid (15.3 g) was added and the reaction mixture was heated at 50° C. for a fisher 5 hours. The reaction mixture was cooled to ambient temperature, methyl t-butylether (55 mL) was added and stirred for 5 minutes. Water (275 mL) was added, the reaction cooled to 0° C. and stirred for 1 hour. The solid was filtered and the reaction flask was washed with MTBE (2×35 mL) and poured over the filtered cake. The solid was dried in a vacuum oven at 60° C. for 10 hours to afford impure title compound as a solid (14 g, 51%) which was used without further purification. A small sample was crystallised from EtOH;

1. temperaturethe reaction mixture was heated at 50° C. for a fisher 5 hours
2. temperatureThe reaction mixture was cooled to ambient temperature
3. temperaturethe reaction cooled to 0° C.
4. stirringstirred for 1 hour
5. filtrationThe solid was filtered
6. washthe reaction flask was washed with MTBE (2×35 mL)
7. additionpoured over the filtered cake
8. customThe solid was dried in a vacuum oven at 60° C. for 10 hours