HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Diisopropylethylamine → HCID 178485964, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 4-Chlorophenyl chloroformate | HCID 139059 | — |
| Edukt | HCID 178484804 | HCID 178484804 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | KHSO4 ether | HCID 86584777 | — |
| Produkt | HCID 178485964 | HCID 178485964 | 117,5% |
Reaktionsschritte
A solution of 1.41 g (corresponds to 3.0 mmol) of trans-Methanesulfonic acid 3-(4-methylamino-cyclohexyl)-prop-2-ynyl ester trifluoroacetate in 20 ml CH2Cl2 was first cooled at 0° C., treated with 0.5 ml (3.6 mmol) 4-chlorophenylchloroformate and then with 2.57 ml (15 mmol; 5 equivalents) of Huenigs base (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 1.41 g (quantitative) of crude trans-Methanesulfonic acid 3-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexyl}-prop-2-ynyl ester, MS: 400 (MH+, 1Cl). The crude product was directly used in the next step.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07335687B2 |
| Quelldatensatz | uspto-grants-2008_02 |
| ORD ID | ord-961ae6a25a3c480a9cb7188510020e34 |
| Quellennotiz | uspto-grants-2008_02 |