HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → 1h-Indole-3-acetonitrile, 6-nitro-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Cyanide | HCID 9032 | — |
| Reactant | 6-Nitrogramine | HCID 23385 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1h-Indole-3-acetonitrile, 6-nitro- | HCID 252385 | 36% |
Reaction Steps
To a mixture of DMF (35 mL) and MeI (74.6 g, 0.53 mol) in water (35 mL) and THF (400 mL) was added dimethyl-(6-nitro-1H-indol-3-ylmethyl)-amine (23 g, 0.105 mol). After the reaction mixture was refluxed for 10 min, potassium cyanide (54.6 g, 0.84 mol) was added and the mixture was kept refluxing overnight. The mixture was then cooled to room temperature and filtered. The filtrate was washed with brine (300 mL×3), dried over Na2SO4, filtered and concentrated. The residue was purified by column chromatography to give (6-nitro-1H-indol-3-yl)-acetonitrile (B-9-a) (7.5 g, 36%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101767B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-18e4f848d6734ac9ba8134c0a65c9709 |
| Source note | uspto-grants-2012_01 |