HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → Ethyl 5,6-Dichloronicotinate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | 5,6-Dichloronicotinic acid | HCID 247987 | — |
| Product | Ethyl 5,6-Dichloronicotinate | HCID 16762519 | — |
Reaction Steps
To a solution of 5,6-dichloronicotinic acid (20.01 g, 104 mmol) in EtOH (500 mL) at 20° C. was added chlorotrimethylsilane (132 mL, 1042 mmol). The reaction was stirred for 72 hours. The reaction mixture was then concentrated and diluted with EtOAc (500 mL), and washed with saturated NaHCO3 (2×100 mL) and brine (100 mL). The organic was then dried (Na2SO4) and concentrated under reduced pressure to give final crude product (21.25 g). LCMS m/z 220.1 (M+H)+, Rt 0.94 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434719B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-5a45f9597fb941b9ae778f44080a3dfb |
| Source note | uspto-grants-2016_09 |