HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → (R)-4-[3-(tert-Butyldimethylsilanyloxy)-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2H-1,4-benzoxazin-3(4H)-one | HCID 72757 | — |
| Reactant | (S)-3-bromo-2-methylpropoxy-tert-butyldimethylsilane | HCID 11032834 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (R)-4-[3-(tert-Butyldimethylsilanyloxy)-2-methylpropyl]-4H-benzo[1,4]oxazin-3-one | HCID 68910127 | 85% |
Reaction Steps
A reaction flask was charged with 4H-Benzo[1,4]oxazin-3-one (1.49 g, 10.0 mmol), (S)-(3-bromo-2-methylpropoxy)-tert-butyldimethylsilane (2.67 g, 10.0 mmol), and Cs2CO3 (4.89 g, 15.0 mmol) in MeCN (15 mL) and stirred at rt for 7 days. The reaction mixture was quenched with water and the product extracted into EtOAc. The combined organic layers were dried over Na2SO4, filtered, and concentrated. The product was purified by flash column chromatography (SiO2; n-heptane/EtOAc 2:1) to give the title compound (2.84 g, 85%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07550459B2 |
| Source dataset | uspto-grants-2009_06 |
| ORD ID | ord-0b27aa920bd943c4bd0c7dcb9ef6c920 |
| Source note | uspto-grants-2009_06 |