Imidazole → HCID 57898847, compound

TBDMSCl (5.22 g) was added to an N,N-dimethylformamide (50 ml) solution of 2,4-dichloro-5-iodophenol (10 g) synthesized according to the production method described in WO 2001/027088 and imidazole (2.83 g), and the resulting mixture was stirred at room temperature for 4 hours. Water (150 ml) was added to the solution, and then extracted with n-hexane (200 ml). Then, the n-hexane solution was sequentially washed twice with water (100 ml) and once with a saturated aqueous sodium chloride solution (100 ml), and dried over anhydrous sodium sulfate. After filtration, the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (developing solvent: n-hexane) to yield pale yellow oily tert-butyl(2,4-dichloro-5-iodophenoxy)dimethylsilane (11.39 g).

1. customsynthesized
2. extractionextracted with n-hexane (200 ml)
3. washThen, the n-hexane solution was sequentially washed twice with water (100 ml) and once with a saturated aqueous sodium chloride solution (100 ml)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. distillationthe solvent was distilled off
7. customThe resulting residue was purified by silica gel column chromatography (developing solvent: n-hexane)

ORD record

ord-80018e13137342038f4c0cd71ac881a9

Source dataset

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08362236B2