HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 3-(Diethylamino)-1-propanol | HCID 12159 | — |
| Edukt | Methanesulfonyl chloride | HCID 31297 | — |
| Edukt | 4-Chloro-3-nitrophenol | HCID 69127 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 2-Chloro-5-(3-diethylamino-1-propoxy)nitrobenzene | HCID 22014731 | 90,7% |
Reaktionsschritte
MsCl (6.0 mmol) was added dropwise at 0° C. to a stirred solution of 3-diethylamino-1-propanol (6.0 mmol), TEA (6.0 mmol) in anhydrous DCM (6 mL), and the mixture was stirred at the same temperature for 10 min, and at room temperature for additional 1 h. After the removal of the solvent in vacuo, the solid residue was mixed with 4-chloro-3-nitrophenol (5.0 mmol), and K2CO3 (10 mmol) in anhydrous DMF (10 mL), following the general procedure III (Step A). The crude product is purified using silica gel column chromatography 5% MeOH/DCM as eluent to yield 2-chloro-5-(3-diethylamino-1-propoxy)nitrobenzene (1.3 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07087632B2 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-a2ee85c640ce4339a5e720ec558b5af4 |
| Quellennotiz | uspto-grants-2006_08 |