Hydrochloric Acid → HCID 123297189, compound

Temperature

-20 °C

In a 2000 ml 3-necked round bottom flask equipped with mechanical stirror and an addition funnel, 1000 ml hexane was added. With the flask was cooled to −20° C. using a dry ice IPA cold bath, 101 g (1.0 mol) dichlorosilane was condensed and dissolved into hexane. With stirring, a mixture of 113 g (1.0 mol) 2,6-dimethylpiperidine and 111 g (1.1 mol) triethylamine was added dropwise to the flask. After the addition was complete, the reaction mixture was stirred at −20° C. for 1 hour, and then let warming up to room temperature. A salt byproduct precipitate of HCl.Et3N was removed by vacuum filtration in a glove bag purging with N2 to prevent the product reacting with the moisture in the air. A GC/MS analysis on the filtrate confirmed the product 2,6-dimethylpiperidinochlorosilane, showing the product with a molecular ion mass of 177 and supporting mass fragment of mass M —CH3 of 162. The solvent hexane was removed by distillation and the product was separated by vacuum distillation. The boiling point was 60° C. at 10 torr. The yield was 66%.

1. additionwas added
2. customcondensed
3. additionwas added dropwise to the flask
4. additionAfter the addition
5. stirringthe reaction mixture was stirred at −20° C. for 1 hour
6. temperaturelet warming up to room temperature
7. customEt3N was removed by vacuum filtration in a glove bag
8. custompurging with N2
9. customThe solvent hexane was removed by distillation
10. customthe product was separated by vacuum distillation

ORD record

ord-75996917812e44469c9f9c83d4c2d4dc

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08993072B2