Chloropentamethyldisilane → HCID 19812441, compound

HRID 373353Notes

Reaction equation

Br[CH:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4].[CH3:8][Si:9]([CH3:15])([CH3:14])[Si:10]([CH3:13])([CH3:12])Cl>[Zn].CN1CCCC1=O>[CH3:12][Si:10]([CH3:13])([CH:2]1[CH2:7][CH2:6][O:5][C:3]1=[O:4])[Si:9]([CH3:15])([CH3:14])[CH3:8]

Participants

Conditions

Temperature: 60 °C

Procedure

200 ml of N-methylpyrrolidone and 34.3 g of zinc dust are placed in a 1,000 ml three-neck flask fitted with internal thermometer, cold-drawn precision glass stirrer and dropping funnel. A mixture of 82.5 g of 2-bromo-γ-butyrolactone and 83.4 g of pentamethylchlorodisilane and 100 ml of N-methylpyrrolidone is added dropwise while stirring so that the internal temperature adjusts to 60° C. during the exothermic reaction. Stirring is continued for a further 6 h at this temperature and the reaction mixture is then poured onto 500 g of flaked ice. Once the ice has melted, the organic phase which separates is separated off and the aqueous phase is extracted with 200 ml of cyclohexane. The combined organic phases are distilled off using a rotary evaporator after drying over magnesium sulfate and the residue is distilled in vacuo.

Workup

customfitted with internal thermometer, cold-drawn precision glass stirrer
additionis added dropwise
stirringStirring
customthe organic phase which separates is separated off
extractionthe aqueous phase is extracted with 200 ml of cyclohexane
distillationThe combined organic phases are distilled off
customa rotary evaporator
dry with materialafter drying over magnesium sulfate
distillationthe residue is distilled in vacuo

Sources & evidence

ORD record: ord-4440e051989445bca1c6b899bbdc701a
Source dataset: uspto-grants-1992_11
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05162559

Reaction notes

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