Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | HCID 58437409 | HCID 58437409 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58437297 | HCID 58437297 | 65.8% |
Reaction Steps
To a solution of 3-formyl-1H-indole-5-carboxylic acid benzyl ester (4.3 g) and pyridine (4.8 g) in tetrahydrofuran (60 ml) was added hydroxylamine hydrochloride (1.6 g) at room temperature and this mixture was stirred at 80° C. overnight. Acetic anhydride was added to reaction mixture at the same temperature and this mixture was stirred for 8 hours. After cooling to ambient temperature, 1 mol/L sodium hydroxide solution (20 mL) was added to this mixture and resulting mixture was extracted with diethyl ether. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and this residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate) to give the title compound (2.8 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08003647B2 |
|---|
| Source dataset | uspto-grants-2011_08 |
|---|
| ORD ID | ord-a5c5129618e64cc2b5e2c39770f172e9 |
|---|
| Source note | uspto-grants-2011_08 |
|---|