HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → N-benzyl-N-methylcarbamoyl chloride
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | N-Methylbenzylamine | HCID 7669 | — |
| Edukt | Triphosgene | HCID 94429 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-benzyl-N-methylcarbamoyl chloride | HCID 10464985 | — |
Reaktionsschritte
At −78° C. pyridine (1.25 mL, 15.5 mmol) followed by methyl benzylamine (2.0 mL, 15.5. mmol) are added to a solution of bis(trichloromethyl) carbonate (1.55 g, 5.2 mmol) in CH2Cl2 (20 mL). The reaction mixture is allowed to warm to RT and stirred for another 1.5 h. For workup 1N HCl is added to the yellow suspension and the mixture is extracted with ethyl acetate. Drying (Na2SO4) of the combined organic exctracts, filtration and evaporation of the solvent affords the title compound. MS (LC-MS): [M+H]+=184.1. tR (HPLC, Waters Symmetry C18 column, 20-95% CH3CN/H2O/3.5 min, 95% CH3CN/H2O, 2 min, CH3CN and H2O containing 0.1% TFA, flow: 0.6 mL/min): 3.84 min.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07807709B2 |
| Quelldatensatz | uspto-grants-2010_10 |
| ORD ID | ord-4142003187f249e9a9d2daa207c288d2 |
| Quellennotiz | uspto-grants-2010_10 |