Tetraethoxysilane → HCID 57894271, compound

Temperature

-30 °C

At first, a mixed solution of 1,4-diiodobenzene (15 g, 45.6 mmol) and a distilled tetrahydrofuran solution (dist.THF: 114 mL) was added dropwise with 2 mol/L of i-PrMgCl (24 mL (solvent: THF), 48 mmol) at −30° C. Then, the resultant mixture was stirred under a nitrogen atmosphere at −30° C. for 5.5 hours to obtain a reaction solution. Subsequently, the reaction solution was added dropwise (3 drops per second) using a cannula into a mixed solution of tetraethoxysilane (TEOS: 60.6 mL, 272 mmol) and dist.THF (90 mL), which was cooled to −30° C. Thereafter, the resultant mixed solution was stirred at −30° C. for one hour, and further stirred at room temperature for 44 hours to obtain a reaction mixture. After that, the obtained reaction mixture was added with ether (100 ml), and washed with distilled water (dist.H2O). Then, the aqueous layer was extracted with ether. The collected organic layers were washed with sat.NaCl, dried with MgSO4), filtered and concentrated to obtain a crude product. Thereafter, the crude product thus obtained was purified by distillation under a reduced pressure (1.5 mmHg, 120° C.), and thereby 4-(triethoxysilyl)iodobenzene was obtained (10.2 g, 61% yield).

1. customto obtain a reaction solution
2. additionSubsequently, the reaction solution was added dropwise (3 drops per second)
3. additionThereafter, the resultant mixed solution
4. stirringfurther stirred at room temperature for 44 hours
5. customto obtain a reaction mixture
6. customAfter that, the obtained reaction mixture
7. washwashed with distilled water (dist.H2O)
8. extractionThen, the aqueous layer was extracted with ether
9. washThe collected organic layers were washed
10. dry with materialNaCl, dried with MgSO4),
11. filtrationfiltered
12. concentrationconcentrated
13. customto obtain a crude product
14. customThereafter, the crude product thus obtained
15. distillationwas purified by distillation under a reduced pressure (1.5 mmHg, 120° C.)

ORD record

ord-e6e45745733d4dd8b9fb4f6d69c75eb0

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07608673B2