HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 178445722, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | (R)-4-(5-bromo-6-hydroxynaphthalen-2-yl)-4-methyloxazolidin-2-one | HCID 67413226 | — |
| Reactant | HCID 178445812 | HCID 178445812 | — |
| Product | HCID 178445722 | HCID 178445722 | 45% |
Reaction Steps
(R)-4-(5-Bromo-6-hydroxy-naphthalen-2-yl)-4-methyl-oxazolidin-2-one (2.16 g, 6.70 mmol) was dissolved in tetrahydrofuran (22.50 mL, 277.4 mmol) in a capped 250 mL round-bottom flask equipped with a magnetic stir bar. trans-4-tert-Butyl-cyclohexanol (2.095 g, 13.41 mmol) and triphenylphosphine (3.517 g, 13.41 mmol) were added and the mixture was stirred for 5 minutes. Diisopropyl azodicarboxylate (2.640 mL, 13.41 mmol) was then slowly added and the reaction mixture was stirred at room temperature overnight. The mixture was concentrated in vacuo, diluted in methylene chloride and adsorbed onto silica gel under reduced pressure, then purified by flash chromatography (0-55% EtOAC in hexanes) to give 1.37 g of the title compound (45% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08546359B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-b7e7314075dc48a78ace7d5760d23bca |
| Source note | uspto-grants-2013_10 |