HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropanol → HCID 66781497, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropanol | HCID 3776 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| Reactant | Methyl 5-nitrosalicylate | HCID 87041 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66781497 | HCID 66781497 | 48.5% |
Reaction Steps
Methyl 2-hydroxy-5-nitrobenzoate (11.82 g, 60 mmol), triphenylphosphine (17.29 g, 66 mmol) and iPrOH (3.96 g, 5 ml, 66 mmol) were taken up in THF (150 ml) and cooled in ice. Di-isopropyl-azodicarboxylate (8.31 g, 10 ml, 66 mmol) was added carefully, and the reaction was stirred at RT overnight. The volatiles were removed in vacuo and the residue treated with EtOAc (50 ml). The solids that didn't dissolve were removed by filtration, and the filtrate evaporated to dryness in vacuo. The residue was purified by column chromatography to give methyl 2-isopropoxy-5-nitrobenzoate (6.92 g, 48.5%) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450506B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-09b3c53ca3f04054919c6b0dd4147ad7 |
| Source note | uspto-grants-2013_05 |