Lithium Hexamethyldisilazide → Hexamethyldisilazane

Compound 7E (14.1 g, 26.4 mmol) in THF (100 mL) was cooled to −78° C. under nitrogen. A solution of LiHMDS (27 mL, 1.0M in THF, 27.0 mmol) was added slowly at −78° C. Upon completion of the addition, the reaction flask was allowed to warm to room temperature. After stirring at room temperature for 2 h, the reaction mixture was concentrated under vacuum and hexane (100 mL) was added. The precipitated lithium salts were filtered off through a Celite pad, rinsed with additional hexane, and the combined filtrates were concentrated under vacuum to give crude bis(trimethylsilyl)amine product 7F (26.4 mmol), which was stored as a stock solution for future use.

1. additionUpon completion of the addition
2. concentrationthe reaction mixture was concentrated under vacuum and hexane (100 mL)
3. additionwas added
4. filtrationThe precipitated lithium salts were filtered off through a Celite pad
5. washrinsed with additional hexane
6. concentrationthe combined filtrates were concentrated under vacuum

ORD record

ord-032030999bc14c6ba31971163b19e3cf

Source dataset

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09101638B2