HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → tert-Butyl [(1R,2S)-2-methoxy-2,3-dihydro-1H-inden-1-yl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Barium hydroxide | HCID 6093286 | — |
| Reactant | Barium Oxide Nanoparticle Dispersion | HCID 9855530 | — |
| Reactant | tert-Butyl ((1R,2S)-2-hydroxy-2,3-dihydro-1H-inden-1-yl)carbamate | HCID 17998891 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | tert-Butyl [(1R,2S)-2-methoxy-2,3-dihydro-1H-inden-1-yl]carbamate | HCID 86614253 | 25% |
Reaction Steps
A mixture of tert-butyl [(1R,2S)-2-hydroxy-2,3-dihydro-1H-inden-1-yl]-carbamate (680. mg, 2.73 mmol), DMF (21.1), barium monoxide (5.02 g, 32.7 mmol), barium hydroxide (2.80 g, 16.4 mmol) and iodomethane (1.70 mL, 27.3 mmol) was stirred overnight. LC/MS showed no starting material. The reaction was quenched via addition of a saturated solution of NaHCO3 and was extracted with DCM. The organic layer was washed with H2O (3×), dried over sodium sulfate and concentrated in vacuo. The residue was purified via silica gel chromatography eluting with a gradient of 0 to 50% EtOAc in hexanes to afford the title compound (178 mg, 25%). LC/MS: Rt=1.24 min, ES+ 264 (AA standard).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08008307B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-8fb34a0c270b42a38a4cc2bd536b20b6 |
| Source note | uspto-grants-2011_08 |