反应详情

温度

-30 °C

To 5.4 g (12.0 mmol) of product 1 and 6.2 g (24 mmol) of product 2 in 135 ml of methylenehloride 8 ml of diisopropylethylamine is added at 10° C. and 4.8 ml of trimethylsilylchloride is added dropwise. After 1 h 14 ml of a 1 molar solution of titantetrachloride in methylenehloride is added dropwise at −10° C. It is stirred for 3 h at −10° C. and further 12 h at −30° C. stored without stirring. Afterwards 8 ml of acetic acid and 140 ml of a 7% aqueous solution of tartratic acid is added and it is stirred for further 2 h at room temperature. After addition of 50 ml of a 20% aqueous solution of sodiumhydrogensulfit it is stirred for another 1 h and extracted with methylenehloride. The organic phase is dried by magnesium sulfate, evaporated and purified by chromatography on silica gel/Ethylacetate/heptane=1/3->1/1. 6.3 g (74%) of product 3 is obtained in form of a light yellow solid compound: C40H47N3O7Si (709.92) MS (ESI+) 710 (M+H+).

1. stirringwithout stirring
2. stirringit is stirred for further 2 h at room temperature
3. stirringis stirred for another 1 h
4. extractionextracted with methylenehloride
5. dry with materialThe organic phase is dried by magnesium sulfate
6. customevaporated
7. custompurified by chromatography on silica gel/Ethylacetate/heptane=1/3->1/1