Dichlorodimethylsilane → HCID 54012527, compound

3-Ethylthiopropyl chloride (7.00 g, 50 mmol) was dropped slowly into Mg turnings (1.22 g, 50 mmol) activated with 2 drops of Br2 in Et2O (70 mL). After 12 h of reflux the Grignard reagent was added to Me2SiCl2 (25.8 g, 200 mmol) in diethyl ether (100 mL). After refluxing for 18 h under mechanical stirring the Mg salts were filtered off, washed with Et2O (2×25 mL), and the solvent was evaporated from the combined filtrates. The residue was fractionally distilled: 45° C./0.01 torr, 4.20 g, 42%.

1. temperatureAfter refluxing for 18 h
2. filtrationwere filtered off
3. washwashed with Et2O (2×25 mL)
4. customthe solvent was evaporated from the combined filtrates
5. distillationThe residue was fractionally distilled
6. custom45° C./0.01 torr, 4.20 g, 42%

ORD record

ord-88a44910d52145e99b1945a6222ab852

Source dataset

uspto-grants-1999_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05876830