HuagongsheHuagongshe Chemistry Print Report · For research reference only
Imidazole → HCID 58994475, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Imidazole | HCID 795 | — |
| Reactant | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Reactant | 2-Methyl-2-(4-nitrophenyl)propan-1-ol | HCID 22249279 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58994475 | HCID 58994475 | 65% |
Reaction Steps
To a mixture of 2-methyl-2-(4-nitro-phenyl)-propan-1-ol (as prepared in the previous step, 1.50 g, 7.68 mmol) and t-butyl-dimethylsilyl chloride (1.51 g, 9.99 mmol) in 60 mL of DCM was slowly added imidazole (3.09 g, 45.4 mmol). After stirring at RT for 16 h, the mixture was treated with 40 mL of DCM and washed with H2O (30 mL), 15% aqueous citric acid (30 mL) and brine (20 mL). The organic layer was dried (Na2SO4) and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (0-5% EtOAc/hexane) to give 1.82 g (65%) of the title compound as a light brown oil. 1H-NMR (CDCl3; 400 MHz): δ 7.85 (d, 2H, J=8.8 Hz), 7.52 (d, 2H, J=8.8 Hz), 3.59 (s, 2H), 1.35 (s, 6H), 0.86 (s, 9H), −0.04 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08674100B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-87c08e3df14945e8bfc5f74dee5a94d4 |
| Source note | uspto-grants-2014_03 |