反应详情

温度

170 °C

In a 50 mL Claisens flask under an argon atmosphere, a mixture of 13.5 g (46.3 mmol) of 33, 20.2 g (97.2 mmol) of Si(OEt)4, and 9.03 g (50.9 mmol) of 2,6-diisopropylaniline was heated to 170° C., and then 0.37 mL of 96% H2SO4 was added. This mixture was stirred at this temperature for 35 hr, and the formed ethanol was slowly distilled off Later, 300 mL of cold water was added, and the product was extracted with 2×100 mL of diethyl ether. The combined extract was dried over K2CO3 and then evaporated to dryness. The product was isolated by flash-chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether, 100:1, vol.). This procedure gave 14.4 g (69%) of 34.

1. distillationthe formed ethanol was slowly distilled off Later
2. addition300 mL of cold water was added
3. extractionthe product was extracted with 2×100 mL of diethyl ether
4. extractionThe combined extract
5. dry with materialwas dried over K2CO3
6. customevaporated to dryness
7. customThe product was isolated by flash-chromatography on silica gel 60 (40-63 um, eluent: from hexanes to hexanes-diethyl ether, 100:1, vol.)