HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → HCID 178485965, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | 4-Chlorophenyl chloroformate | HCID 139059 | — |
| Edukt | HCID 178484806 | HCID 178484806 | — |
| Lösungsmittel | Hexamethyldisilazane | HCID 13838 | — |
| Produkt | HCID 178485965 | HCID 178485965 | — |
Reaktionsschritte
4.60 g (32.14 mmol) of trans-(4-Methylamino-cyclohexyl)-methanol was suspended in 85 ml hexamethyldisilazane and refluxed for 5 h. The solution was evaporated under reduced pressure and dissolved in 50 ml THF. 6.14 g (32.14 mmol) of 4-chlorophenylchloroformate were added slowly at 0° C. and stirred for 16 h at room temperature. 30 ml H2O were added and after 1 h the solvents were evaporated. The residue was extracted with water/Et2O (3×), the organic phases were washed with 10% NaCl, dried over Na2SO4 and evaporated to yield after flash-chromatography on silica gel (hexane/EtOAc 4:1 to 1:1) 5.48 g (57%) of trans-(4-Hydroxymethyl-cyclohexyl)-methyl-carbamic acid 4-chloro-phenyl ester, MS: 298 (MH+, 1Cl).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06858651B2 |
| Quelldatensatz | uspto-grants-2005_02 |
| ORD ID | ord-d6ce6f00a8b94d138694ffea83c0e1e0 |
| Quellennotiz | uspto-grants-2005_02 |