Hydrogen Bromide → HCID 11983794, compound

Temperature

0 °C

Under a nitrogen atmosphere, 16.3 g (0.06 mol) of di(4-chlorophenyl)sulfoxide was dissolved in 250 ml dichloremethane. Into the resulting solution kept at 0 to 5° C., 10.8 g (0.10 mol) of trimethylchlorosilane was added dropwise; the mixture was stirred at 0° C. for 30 min. Thereafter, 200 g of a tetrahydrofuran (THF) solution of the Grignard reagent prepared by the usual process with 4-bromochlorobenzene (0.18 mol) was added dropwise over the period of 30 min into the reaction vessel cooled with 0 to 10° C. ice water. After agitated for one hr at 0° C., followed by another hr agitation at room temperature, the reaction solution was slowly poured into an aqueous solution containing 250 ml of an aqueous 12% hydrogen bromide solution and ice, then extracted with 250 ml dichloromethane. The extract was dried with sodium sulfate.

1. customkept at 0 to 5° C.
2. additionwas added dropwise over the period of 30 min into the reaction vessel
3. stirringAfter agitated for one hr at 0° C.
4. waitfollowed by another hr
5. additionagitation at room temperature, the reaction solution was slowly poured into an aqueous solution
6. extractionextracted with 250 ml dichloromethane
7. dry with materialThe extract was dried with sodium sulfate

ORD record

ord-ce97125950ee49cb92d2c881177bc3e6

Source dataset

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08110337B2