HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 24992432, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 67019941 | HCID 67019941 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 24992432 | HCID 24992432 | — |
Reaction Steps
The product obtained in Step A (127 mg, 0.23 mmol) was dissolved in DMSO (2 mL). NaH (20 mg, 0.51 mmol) was added and the reaction was stirred at rt for 1 h. The reaction was diluted with EtOAc and washed with a saturated NaHCO3 solution, 10% NaHSO4, brine, dried (Na2SO4), filtered and concentrated The residue was purified by flash chromatography on silica gel gradient eluted with 0-70% EtOAc in hexane to afford Example 113. Further purification on an AD column, eluting with 12% IPA/heptane provided the two pure enantiomers indicated below:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07999107B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-8b90cdfa4e5140a68f792794af86ca75 |
| Source note | uspto-grants-2011_08 |