HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Chloropyridazine-4-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | Ethyl 3-chloropyridazine-4-carboxylate | HCID 14542887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-Chloropyridazine-4-carboxylic acid | HCID 21780772 | 94.2% |
Reaction Steps
To a solution of crude 3-chloro-pyridazine-4-carboxylic acid ethyl ester (565 mg) in THF (5 ml) was added 2N LiOH (3.03 ml, 6.06 mmol) and the mixture was stirred for 15 min at ambient temperature. The pH of the reaction mixture was then adjusted to 2 by addition of 0.1N HCl and the mixture was extracted five times with ethyl acetate. The combined extracts were dried (Na2SO4) and evaporated to give the crude title compound as a brown solid (452 mg, 94%) which was used in the next reaction step without further purification. 1H NMR (d6-DMSO): 8.07 (d, J=5 Hz, 1H), 9.41 (d, J=5 Hz, 1H), 14.52 (s br, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928106B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-824b4cce6b7f4bc08ffb9369b1e89944 |
| Source note | uspto-grants-2011_04 |