反应详情

温度

75 °C

Silanol fluid, Rhone Poulenc 48V3500, (0.092 eq OH) was stirred under nitrogen and warmed to 70° C. with triethylamine-dimethylaminopyridine (1.05 eq, 1% DMAP by weight). The product of example 2 (0.0956 eq, 20.5 g) was added. The reaction mixture was stirred at 75° C. for three hours then methanol (50 g) was added slowly. After one hour, volatiles were removed by concentration on a rotary evaporator, the reaction mixture was diluted with hexane and filtered through diatomaceous earth. Removal of solvent on a rotary evaporator at 75° C. (0.1 mm Hg) gave the product: Viscosity 4680 cps, GPC MWwt 30787, MWnumber 23943.

1. waitAfter one hour
2. customvolatiles were removed by concentration on a rotary evaporator
3. additionthe reaction mixture was diluted with hexane
4. filtrationfiltered through diatomaceous earth
5. customRemoval of solvent
6. customon a rotary evaporator at 75° C. (0.1 mm Hg)
7. customgave the product