HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22473459, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 10154435 | HCID 10154435 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22473459 | HCID 22473459 | 92% |
Reaction Steps
To a mixture of 6-(3-carbomethoxyphenyl)-5-cyano-3,6-dihydro-4-methyl-2-oxo-1-(2H)-pyrimidinecarboxylic acid, 1-ethyl amide (0.34 g, 1.0 mmol), MeOH (9 mL) and water (3 mL) at 0° C. was added lithium hydroxide (0.84 g, 20.0 mmol). The reaction mixture was stirred for 1 h, acidified to pH 2 with 1 N HCl and extracted with EtOAc. The extract was dried (MgSO4) and concentrated in vacuo to give 6-(3-carboxyphenyl)-5-cyano-3,6-dihydro-4-methyl-2-oxo-1-(2H)-pyrimidinecarboxylic acid, 1-ethyl amide as a colorless solid (0.30 g, 92%): 1H NMR (MeOH-d4, 400 MHz) δ 8.98 (s, 1H), 7.89 (m, 2H), 7.46 (d, 1H, J=7.5 Hz), 7.42 (t, 1H, J=7.5 Hz), 6.12 (s, 1H), 3.16 (m, 2H), 2.06 (s, 3H), 1.03 (t, 3H, J=7.0 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06900214B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-68b3d92dbaf5454c96eecb27b25b998c |
| Source note | uspto-grants-2005_05 |