HuagongsheHuagongshe Chemistry Print Report · For research reference only
Perchloric Acid → HCID 70855555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Perchloric Acid | HCID 24247 | — |
| Reactant | HCID 70855549 | HCID 70855549 | — |
| Solvent | tert-Butyl acetate | HCID 10908 | — |
| Product | HCID 70855555 | HCID 70855555 | 149.4% |
Reaction Steps
Under a nitrogen atmosphere, perchloric acid (70%, 1.33 mL) was added at −10° C. to a solution of methyl (3-bromo-4-methyl-benzo[b]thiophen-2-yl)-hydroxy-acetate (23h) (250 mg, 0.79 mmol) in tert-butyl acetate (10 mL). After 1 hour, the reaction was quenched with a saturated aqueous solution of sodium bicarbonate and extracted with dichloromethane (2×30 mL). The organic layer was washed with brine (20 mL), dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by flash chromatography on silica gel (cyclohexane/ethyl acetate 90/10) to afford the desired product (23i) as a white solid (220 mg, 0.59 mmol, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09238026B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-15227b860f074c65bafd6ae8135cd30a |
| Source note | uspto-grants-2016_01 |