Triethylamine → HCID 13033313, compound

At first, 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 dimethylformamide (DMF: 26 mL) and triethylamine (2.56 mL, 18.4 mmol). Then, triethoxysilane (1.87 mL, 10.1 mmol) was added dropwise thereto at 0° C. The resultant mixture was stirred under a nitrogen atmosphere at 80° C. for one hour to obtain a reaction mixture. Subsequently, a solvent in the reaction mixture was distilled with a vacuum pump. Under a nitrogen atmosphere, the residue was extracted with ether, filtered with celite, and concentrated to obtain a crude product. Thereafter, the crude product thus obtained was purified by Kugel distillation, and thereby 4-bromo-triethoxysilylbenzene was obtained (2.38 g, 81% yield).

1. customat 0° C
2. customto obtain a reaction mixture
3. distillationSubsequently, a solvent in the reaction mixture was distilled with a vacuum pump
4. extractionUnder a nitrogen atmosphere, the residue was extracted with ether
5. filtrationfiltered with celite
6. concentrationconcentrated
7. customto obtain a crude product
8. customThereafter, the crude product thus obtained
9. distillationwas purified by Kugel distillation

ORD record

ord-27c1b379d735480aa22a61d061c7fa07

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07608673B2