HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2,6-Lutidine → N-(cyanomethyl)-2-hydroxy-4-methoxy-N-methylbenzamide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2,6-Lutidine | HCID 7937 | — |
| Edukt | Acetonitrile, 2-(methylamino)- | HCID 36652 | — |
| Edukt | 2-Hydroxy-4-methoxybenzoyl chloride | HCID 23118559 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-(cyanomethyl)-2-hydroxy-4-methoxy-N-methylbenzamide | HCID 55207279 | — |
Reaktionsschritte
To a solution of 2-hydroxy-4-methoxybenzoyl chloride (22.19 g, 118.9 mmol) in 500 CH2Cl2 were added (methylamino)acetonitrile (10 g, 142.7 mmol) and 2,6-lutidine (19.1 g, 178.4 mmol). The reaction was stirred at rt overnight. The reaction mixture was then partitioned between EtOAc and 1(N) aq HCl. Organic layer washed with 1(N) aq HCl (2×), dried over Na2SO4 and concentrated to light yellow viscous material (24.63 g, 94%). This material was used in the next step without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07691879B2 |
| Quelldatensatz | uspto-grants-2010_04 |
| ORD ID | ord-337927e2294b41c7ba3c1c1f19860c77 |
| Quellennotiz | uspto-grants-2010_04 |