HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloronicotinoyl chloride → HCID 118492328, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloronicotinoyl chloride | HCID 2774541 | — |
| Reactant | HCID 118492320 | HCID 118492320 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 118492328 | HCID 118492328 | 57.9% |
Reaction Steps
3-ethoxy-3-carbonylpropionic acid (13.2 g, 100 mmol) was dissolved in tetrahydrofuran (100 mL), n-butyl lithium (25.6 g, 400 mmol) was added dropwise at −78° C., reacted at low temperature for 1 h, 2-chloronicotinoyl chloride (17.5 g, 99.4 mmol) in tetrahydrofuran (20 mL) solution was added, and continuously reacted at low temperature for 3 h. After reaction was complete, extraction was performed with water/dichloromethane, organic phase was rotated for dryness, and separated by column chromatography to obtain product 13.8 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181244B1 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-59e11d1444da4ec3a7bdb751cca23c62 |
| Source note | uspto-grants-2015_11 |