HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane → 4-(3-Chloro-4-methoxybenzylamino)-5-(2-benzyloxyethoxycarbonyl)-6-chloro-2-methylthiopyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | 2-(Benzyloxy) ethanol | HCID 12141 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 4-(3-Chloro-4-methoxybenzylamino)-5-chloroformyl-6-chloro-2-methylthiopyrimidine | HCID 17848283 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 4-(3-Chloro-4-methoxybenzylamino)-5-(2-benzyloxyethoxycarbonyl)-6-chloro-2-methylthiopyrimidine | HCID 17848357 | — |
Reaktionsschritte
A mixture of whole amount of 4-(3-chloro-4-methoxybenzylamino)-5-chloroformyl-6-chloro-2-methylthiopyrimidine (prepared in the above (1)), methylene chloride 15 ml and 2-benzyloxyethanol 224 mg is refluxed for 30 minutes. After cooling the reaction mixture is diluted with water and neutralized with an aqueous saturated sodium hydrogen carbonate solution. The solution is washed with ethyl acetate. The methylene chloride layer is diluted with ethyl acetate, washed, dried and concentrated in vacuo. The residue is separated with silica gel chromatography (solvent; hexane:ethyl acetate=5:1) to give 4-(3-chloro-4-methoxybenzylamino)-5-(2-benzyloxyethoxycarbonyl)-6-chloro-2-methylthiopyrimidine as a colorless oil 655 mg.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07273868B2 |
| Quelldatensatz | uspto-grants-2007_09 |
| ORD ID | ord-80a90dea63d84750ada52c2c43e0d574 |
| Quellennotiz | uspto-grants-2007_09 |