Triethylamine → HCID 13033313, compound

Temperature

80 °C

Firstly, a mixture of 4-iodo-bromobenzene (2.60 g, 9.19 mmol), t-butylammoniumiodido (3.39 g, 9.18 mmol) and [Rh(cod) (CH3CN)2] (105 mg, 0.277 mmol) was added with DMF (26 mL) and triethylamine (2.56 mL, 18.4 mmol). Triethoxysilane (1.87 mL, 10.1 mmol) was added dropwise to the resultant mixture at 0° C., and then the mixture thus newly produced was stirred under a nitrogen atmosphere at 80° C. for 1 hour to obtain a reaction mixture. Subsequently, the solvent in the reaction mixture was distilled away with a vacuum pump, and then the resultant mixture was subjected to a celite filtration process with ether and a concentration process under a nitrogen atmosphere to obtain a crude product. The obtained crude product was purified with a Kugelrohr distillation apparatus to obtain 4-bromo-triethoxysilylbenzene (2.38 g, 81% yield).

1. customthe mixture thus newly produced
2. customto obtain a reaction mixture
3. distillationSubsequently, the solvent in the reaction mixture was distilled away with a vacuum pump
4. customa concentration process under a nitrogen atmosphere to obtain a crude product
5. customThe obtained crude product
6. distillationwas purified with a Kugelrohr distillation apparatus

ORD record

ord-1a08c300753c4e3e9129c5455a24d916

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08053588B2