HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl formate → 2-(2-Chloropyridin-3-yl)-3-oxopropanenitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl formate | HCID 8025 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-(2-Chloropyridin-3-yl)acetonitrile | HCID 14739543 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-(2-Chloropyridin-3-yl)-3-oxopropanenitrile | HCID 86614161 | — |
Reaction Steps
A solution of 2-(2-chloropyridin-3-yl)acetonitrile (2.0 g, 13 mmol) in THF (5 mL) was slowly added to a suspension of sodium hydride, 60% in mineral oil (1.31 g, 33.0 mmol) in THF (10 mL) at 0° C. The mixture was stirred for 15 minutes, and ethyl formate (1.1 mL, 13 mmol) was slowly added. The mixture was stirred at RT, and monitored by LCMS. Upon completion, the reaction was extracted into EtOAc, washed organics 2×H2O, dried with Mg2SO4, filtered through fritted funnel, and lyophilized to yield 2-(2-chloropyridin-3-yl)-3-oxopropanenitrile as reddish brown solid. The crude was used without further purification. MS m/z=181 [M+1]+. Calc'd for C8H5ClN2O: 180.59.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07560551B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-7a34f32bc73c4237af0cd8780b107316 |
| Source note | uspto-grants-2009_07 |