HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 57426190, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | tert-Butyl bromoacetate | HCID 79177 | — |
| Reactant | 1H-Indole-3-acetonitrile, 4-nitro- | HCID 10954595 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 57426190 | HCID 57426190 | — |
Reaction Steps
Sodium hydride (198 mg of a 60% dispersion in mineral oil, 5.0 mmol) was added to a solution of (4-nitro-1H-indol-3-yl)acetonitrile from Step B (910 mg, 4.52 mmol) in DMF (15 mL). After 10 min, tert-butyl bromoacetate (0.801 mL, 5.4 mmol) was added dropwise and the reaction mixture was stirred at ambient temperature for 1.5 h. The mixture was partitioned between H2O (50 mL) and EtOAc (100 mL) and the organic extract was washed with brine, dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by silica gel chromatography, eluting with a gradient of hexane:EtOAc—100:0 to 0:100, to give the title compound. MS: m/z=316 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696192B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-5a660c1785e1491692de9994e0ad8009 |
| Source note | uspto-grants-2010_04 |