HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 178457232, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-Chlorophenyl chloroformate | HCID 139059 | — |
| Edukt | HCID 178457231 | HCID 178457231 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Lösungsmittel | Ether sodium bicarbonate | HCID 23682952 | — |
| Produkt | HCID 178457232 | HCID 178457232 | 67,2% |
Reaktionsschritte
A solution of 66 mg (0.3 mmol) of trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-amine in 0.3 ml dioxane was treated with 0.103 ml (0.6 mmol; 2 equivalents) Huenig's base and dropwise with a solution of 0.042 ml (0.27 mmol) 4-chlorophenylchloroformate in 0.16 ml dioxane (during 10 min). After 5 min at RT, the mixture was dissolved in aqueous saturated NaHCO3/Et2O (3×). The organic phase was dried over Na2SO4 and evaporated. Flash column chromatography on silica gel with CH2Cl2/MeOH (99:1 to 97:3) yielded 68 mg (61%) of trans-{4-[3-(Allyl-methyl-amino)-prop-1-ynyl]-cyclohexyl}-methyl-carbamic acid 4-chloro-phenyl ester, MS: 375 (MH+, 1Cl).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06858651B2 |
| Quelldatensatz | uspto-grants-2005_02 |
| ORD ID | ord-e00da6cf44d6447186086da1eba9ec4a |
| Quellennotiz | uspto-grants-2005_02 |