Dichlorosilane → HCID 123297189, compound

To a solution of 7.55 g (66.68 mmol) cis-2,6-dimethylpiperidine in 50 mL of THF at −78° C. was drop-wise added 28.00 mL (70.02 mmol) of a 2.5M solution of n-butyllithium in hexanes. A precipitate evolved and the reaction mixture was warmed to room temperature while stirring. After one hour this mixture was added drop-wise to a solution of 6.74 g (66.68 mmol) dichlorosilane in 30 mL xylenes and 70 mL hexanes at −40° C. and a light gray precipitate formed. The reaction mixture was stirred for 16 hours after which it was decanted from the evolved solid and subjected to distillation at ambient pressure to remove volatiles. 3.16 g of desired product was isolated with a yield of 27%. The product was confirmed by GC/MS analysis as 2,6-Dimethylpiperidinochlorosilane.

1. customa light gray precipitate formed
2. stirringThe reaction mixture was stirred for 16 hours after which it
3. customwas decanted from the evolved solid
4. distillationsubjected to distillation at ambient pressure
5. customto remove volatiles

ORD record

ord-4a056da451984f838881109460b44d02

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08993072B2