HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dichloromethane → (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dichloromethane | HCID 6344 | — |
| Edukt | Methyl triflate | HCID 9526 | — |
| Edukt | 3-Cyano-4-dimethylamino-benzoic acid methyl ester | HCID 59847657 | — |
| Lösungsmittel | Diethyl Ether | HCID 3283 | — |
| Produkt | (2-Cyano-4-methoxycarbonyl-phenyl)-trimethyl-ammonium trifluoro-methanesulfonate | HCID 86621519 | 69% |
Reaktionsschritte
To a stirred solution of 6.16 g (30.2 mmol) 2c and 110 ml dichloromethane were added 50.0 g (302 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was stirred over night and diethylether was added. After evaporation of one third of the solvent volume the desired compound precipitates and the rest of the solvent was decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water-gradient 1:99 to 80:20). The desired compound 2d was obtained in 69% yield (20.8 mmol, 7.68 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08557776B2 |
| Quelldatensatz | uspto-grants-2013_10 |
| ORD ID | ord-086836f12dc5462394ad3103395aa1e4 |
| Quellennotiz | uspto-grants-2013_10 |