Lithium Hexamethyldisilazide → Hexamethyldisilazane

Chloro intermediate XL (260 mg, 0.48 mmol) in THF (4 mL) was cooled to −78° C. under nitrogen. A solution of 1M LiHMDS solution in THF (0.5 mL, 0.5 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 16 h, the reaction mixture was concentrated under vacuum and hexane (20 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 XLI.

1. additionUpon completion of the addition
2. concentrationthe reaction mixture was concentrated under vacuum and hexane (20 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-e3537725482f4fe18b65ab1dcec2c7db

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09012491B2