HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 22050084, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 5-{[3-bromo-4-[(2,4-difluorobenzyl)oxy]-6-methyl-2-oxopyridin-1(2H)-yl]methyl}pyrazine-2-carboxylate | HCID 22050032 | — |
| Product | HCID 22050084 | HCID 22050084 | 77% |
Reaction Steps
A suspension of ethyl 5-{[3-bromo-4-[(2,4-difluorobenzyl)oxy]-6-methyl-2-oxopyridin-1(2H)-yl]methyl}pyrazine-2-carboxylate (0.18 g, 0.002 mol) and 1N NaOH (0.6 mL in 1:1 v/v EtOH/Water) was stirred at room temperature for 1.5 h. The reaction mixture was acidified with 5% citric acid and filtered the precipitate. It was washed with water, followed by ethanol and dried in vacuo to afford the title compound (0.14 g, 77%) as a light brown powder: 1H NMR (CD3OD/400 MHz)=δ 9.03 (s. 1H), 8.60 (s, 1H), 7.61 (m. 1H), 7.00 (m, 2H), 6.52 (s, 1H), 5.51 (s, 2H), 5.30 (s. 2H), and 2.52 (s, 3H); 19F NMR (CD3OD/400 MHz)=δ−111.75 (m) and −116.06 (m); ES-HRMS m/z 466.0209 (M+H C19H15N4O3BrF2 requires 466.0209).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07067540B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-cf3ea63f50ec407c875e6909d8083aaa |
| Source note | uspto-grants-2006_06 |