Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | 2,4-Dichloro-5-iodophenol | HCID 57749478 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57898847 | HCID 57898847 | 81.6% |
Reaction Steps
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).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08362236B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-80018e13137342038f4c0cd71ac881a9 |
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| Source note | uspto-grants-2013_01 |
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