反应详情

温度

170 °C

In a 50 mL Claisens flask under argon atmosphere, a mixture of 10.6 g (46.3 mmol) of 29, 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 for 5 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: hexanes and then hexanes-diethyl ether, 100:1, vol.). The isolated product was additionally washed with 3×30 mL hexanes and dried in vacuum. This procedure gave 14.7 g (82%) of yellowish solid.

1. distillationthe formed ethanol was slowly distilled off
2. additionLater, 300 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
8. washThe isolated product was additionally washed with 3×30 mL hexanes
9. customdried in vacuum