HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Pyridine → HCID 178485835, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Pyridine | HCID 1049 | — |
| Edukt | 4-Chlorophenyl Isocyanate | HCID 7693 | — |
| Edukt | HCID 178484804 | HCID 178484804 | — |
| Lösungsmittel | 1,4-Dioxane | HCID 31275 | — |
| Lösungsmittel | KHSO4 ether | HCID 86584777 | — |
| Produkt | HCID 178485835 | HCID 178485835 | 101,9% |
Reaktionsschritte
A solution of 1.38 g (corresponds to 3.0 mmol) of trans-Methanesulfonic acid 3-(4-methylamino-cyclohexyl)-prop-2-ynyl ester trifluoroacetate in 7 ml dioxane was first cooled to 8° C., treated with 0.69 g (4.5 mmol) 4-chlorophenyl isocyanate and then with 1.2 ml (15 mmol; 5 equivalents) of pyridine (during 3 min). After 45 min at RT, the mixture was dissolved in aqueous 10% KHSO4/Et2O (3×). The organic phases were washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated to give 1.22 g (quantitative) of crude trans-Methanesulfonic acid 3-{4-[3-(4-chloro-phenyl)-1-methyl-ureido]-cyclohexyl}-prop-2-ynyl ester, MS: 398 (MH+, 1Cl). The crude product was directly used in the next step.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06858651B2 |
| Quelldatensatz | uspto-grants-2005_02 |
| ORD ID | ord-28db14751ac646c88829af2b73dfd95f |
| Quellennotiz | uspto-grants-2005_02 |