Hexamethyldisilazane → HCID 14949187, compound

Temperature

120 °C

A glass reactor equipped with a stirrer, reflux condenser and gas inlet was charged with hexamethyldisilazane (0.4235 mol, 91.2 ml) and 3-chloropropanesulfonyl chloride (0.4193 mol, 75.0 g). The contents of the reactor were heated. A refluxing liquid was first observed at a temperature of 85°-95° C., and the mixture became clear. The mixture became cloudy at a temperature of about 105 degrees. The temperature of the mixture was maintained at 120° C. for 90 minutes and at 145°-150° C. for 15 minutes. The mixture was then allowed to cool to room temperature, at which time it was filtered, the solids were washed with benzene, and the washing liquid combined with the liquid portion of the mixture. The combined liquids were then heated at 60°-65° C. under reduced pressure to remove volatile materials and then distilled. The fraction boiling from 127°-129° C. under a pressure of from 0.04-0.07 mm. Hg was collected, and was equivalent to a 72.5 % yield based on initial reactants. The 1H NMR spectrum was consistent with the expected product.

1. customA glass reactor equipped with a stirrer
2. temperaturereflux condenser and gas inlet
3. temperatureThe contents of the reactor were heated
4. customwas first observed at a temperature of 85°-95° C.
5. customat a temperature of about 105 degrees
6. temperatureto cool to room temperature, at which time it
7. filtrationwas filtered
8. washthe solids were washed with benzene
9. temperatureThe combined liquids were then heated at 60°-65° C. under reduced pressure
10. customto remove volatile materials
11. distillationdistilled
12. customboiling from 127°-129° C. under a pressure of from 0.04-0.07 mm. Hg
13. customwas collected

ORD record

ord-9549fc4ce46e48f7a268f21976268f1c

Source dataset

uspto-grants-1993_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05194557