HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → Ethyl 4-amino-5-mesityl-1-methyl-1H-pyrazole-3-carboxylate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Methylhydrazine | HCID 6061 | — |
| Edukt | HCID 178418386 | HCID 178418386 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | Ethyl 4-amino-5-mesityl-1-methyl-1H-pyrazole-3-carboxylate | HCID 15516666 | 78,9% |
Reaktionsschritte
To a solution of the product of step B (4.0 g, 13.8 mmol) and 1.6 mL of 12N hydrochloric acid in 100 mL of methanol was added dropwise 0.63 g of methyl hydrazine at 0° C. The reaction mixture was stirred at room temperature 4 hours, and then concentrated. The resulting residue was partitioned between water and ethyl acetate. The organic phase was separated and washed once with brine. The ethyl acetate solution was then mixed with 100 mL of water. Solid Na2S2O4 in excess was added in small portion until TLC showed completion of the reduction. The organic phase was separated, washed with water and brine, and dried over Na2SO4. Evaporation gave 3.1 g of the title compound as a foam.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05723608 |
| Quelldatensatz | uspto-grants-1998_03 |
| ORD ID | ord-75a3caa0644f40ee90d13cb00258ca5f |
| Quellennotiz | uspto-grants-1998_03 |