HCID 21259639, compound → HCID 123309382, compound
Reaction equation
Cl[Si:2]([Cl:12])([Cl:11])[CH2:3][CH:4]([CH2:9][CH3:10])[CH2:5][CH2:6][CH2:7][CH3:8].[CH2:13]([Mg]Br)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]>O1CCCC1.C(OCC)C>[Cl:12][Si:2]([Cl:11])([CH2:3][CH:4]([CH2:9][CH3:10])[CH2:5][CH2:6][CH2:7][CH3:8])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 0 °C
Procedure
Trichloro(2-ethylhexyl)silane (synthesized in accordance with J. Am. Chem. Soc. 2008, 130, 16144-16145, 24.8 g) was placed in a 300 mL four-necked flask in a nitrogen atmosphere, and dissolved in tetrahydrofuran (100 mL). The resulting solution was cooled to 0° C., and a solution of n-octyl magnesium bromide in diethyl ether (Sigma-Aldrich Co. LLC., 2.00 M, 50.0 mL) was added dropwise. The reaction solution was agitated for about 30 minutes at 7° C., and then agitated for about 3 hours at room temperature. The solvent was then distilled off with an evaporator. Hexane was added to the resulting crude product, which was then filtered, after which the solvent was again distilled off. Finally, distillation purification (111° C., 0.61 torr) was performed to obtain the target dichloro(2-ethylhexyl)n-octylsilane (Compound G6, 15.9 g, yield 49%).
Workup
- stirringagitated for about 3 hours at room temperature
- distillationThe solvent was then distilled off with an evaporator
- additionHexane was added to the resulting crude product, which
- filtrationwas then filtered
- distillationafter which the solvent was again distilled off
- distillationFinally, distillation purification (111° C., 0.61 torr)
Sources & evidence
- ORD record
- ord-2cf1bedd3e04462bbb711e39f6b5ece0
- Source dataset
- uspto-grants-2016_02
- Patent number
- US09249257B2
Reaction notes
Loading…