HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59749551, compound → HCID 68773320, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59749551 | HCID 59749551 | — |
| Reactant | HCID 178418689 | HCID 178418689 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68773320 | HCID 68773320 | 98% |
Reaction Steps
A solution of (2,3-dihydro-benzo[1,4]dioxin-5-yl)-(1-trityl-1H-imidazol-4-yl)-methanone (Intermediate B1) (0.91 g, 1.93 mmol) in THF (80 mL) at −10° C. was treated with MeMgBr (2.6 mL, 7.68 mmol of a 3M solution in Et2O) for 45 m. The mixture was quenched with a sat. solution of NH4Cl and water. The layers were separated and the organic layer dried over MgSO4. The suspension was filtered and evaporated to dryness. The material was purified by chromatography on SiO2 with 50% EtOAc in CHCl3 to give 1-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-1-(1-trityl-1H-imidazol-4-yl)-ethanol as a foam 0.95 g (98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07396849B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-b43316dc28064edd95bfc0153ba4fe2a |
| Source note | uspto-grants-2008_07 |