HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Methyl-2-butene → HCID 68672018, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Methyl-2-butene | HCID 10553 | — |
| Reactant | Sodium Chlorite | HCID 23668197 | — |
| Reactant | Monosodium phosphate | HCID 23672064 | — |
| Reactant | HCID 86647620 | HCID 86647620 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68672018 | HCID 68672018 | 117.6% |
Reaction Steps
N-[5-(3,5-Difluoro-benzyl)-1-trityl-1H-indazol-3-yl]-2-fluoro-5-formyl-benzamide (88 mg, 0.135 mmol) in tert-butanol (1.8 mL) at room temperature was treated first with 2-methyl-2-butene (0.079 mL, 1.082 mmol) and then with sodium chlorite (37 mg, 0.405 mmol) and sodium dihydrogenphosphate in water (0.8 mL) drop-wise. The reaction was stirred over-night, EtOAc was then added (30 mL) and washed with water (25 mL). The aqueous layer was extracted twice with EtOAc (2×10 mL). The combined organic layers were washed with brine, evaporated to dryness to leave 106 mg of title compound which was employed in the following step with no need of further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029356B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-48147f3b10fa4cb4b3849c3c3f67a363 |
| Source note | uspto-grants-2015_05 |