HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 2-(2,4-Dimethoxybenzylamino)nicotinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloronicotinonitrile | HCID 81079 | — |
| Reactant | 2,4-Dimethoxybenzylamine | HCID 597250 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | 2-(2,4-Dimethoxybenzylamino)nicotinonitrile | HCID 22293175 | 72.2% |
Reaction Conditions
| Temperature | 80 °C |
|---|
Reaction Steps
2,4-Dimethoxybenzylamine (2.90 g, 17.3 mmol) and triethylamine (1.75 g, 17.3 mmol) were added sequentially to a solution of 2-chloronicotinonitrile (2.0 g, 14.4 mmol) in N,N-dimethylacetamide (29 mL). The reaction was heated at 80° C. for 4 h, quenched with water and extracted with diethyl ether (3×). The combined organic extracts were washed water, saturated brine, dried over magnesium sulfate and concentrated. The crude product was purified by flash chromatography (silica gel, 0-5% ethyl acetate (with 0.1 triethylamine) in dichloromethane gradient elution) to produce the title compound (2.80 g). MS 270.3 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07745427B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-8d936463582b49538798f5c256ddebf8 |
| Source note | uspto-grants-2010_06 |