Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Sulfite | HCID 24437 | — |
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | (R)-tert-butyldimethyl(1-methylcyclohex-2-enyloxy)silane | HCID 68008146 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86667431 | HCID 86667431 | — |
Reaction Steps
3-chlorobenzenecarboperoxoic acid (2.47 g, 11.00 mmol) was added in one portion to a stirred solution of (R)-tert-butyldimethyl(1-methylcyclohex-2-enyloxy)silane, 50b, (1.98 g, 8.87 mmol) and sodium hydrogen carbonate in 30 mL of dry dichloromethane at room temperature under nitrogen. The resulting mixture was stirred for 20 hours. Then, 25% sodium sulfite solution (30 mL) was added and the resulting biphasic mixture was stirred for 15 minutes. The 2 layers were separated and the aqueous layer was extracted with dichloromethane (2×20 mL). The combined organic phases were washed with aqueous saturated NaHCO3, dried (Na2SO4) and concentrated in vacuo. The crude residue was purified by silica gel chromatography (0-10% EtOAc-hexanes gradient) to provide 647 mg of compound 50c.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09345708B2 |
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| Source dataset | uspto-grants-2016_05 |
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| ORD ID | ord-55abc5a7014c4b61be0f3b49d3ded358 |
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| Source note | uspto-grants-2016_05 |
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