HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 54264503, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 592440 | HCID 592440 | — |
| Product | HCID 54264503 | HCID 54264503 | — |
Reaction Steps
3-(1-Methylpyrazol-4-yl)acrylic acid (86.8 g) was added to a solution of sulphuric acid (20 ml) in methanol (690 ml), and the mixture refluxed for 2.5 hours, cooled, then poured onto ice. The acid was neutralised with aqueous sodium hydroxide and the product extracted into dichloromethane, which was dried and evaporated. Crystallisation from ether/petrol gave methyl 3-(1-methylpyrazol-4-yl)acrylate (89.0 g). 1H-NMR (d6-DMSO) δ 3.77 (3H,s), 3.91 (3H,s), 6.16 (1H,d), 7.54 (1H,s), 7.56 (1H,d), 7.69 (1H,s). (APCI) found (M+H)=167. C8H10N2O2 requires 166.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07115616B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-bf5a101ed2c74125ae4f21d014e383df |
| Source note | uspto-grants-2006_10 |