HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Carbonate → (R)-1-tert-butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1-Chloropinacolone | HCID 83572 | — |
| Edukt | (R)-(-)-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 12043264 | — |
| Katalysator | Potassium Iodide | HCID 4875 | — |
| Katalysator | Tetrabutylammonium Bromide | HCID 74236 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | (R)-1-tert-butylcarbonylmethyl-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 12043265 | 99,8% |
Reaktionsschritte
To a solution of 50 g of (R)-(−)-2-oxo-3-tert-butoxycarbonylamino-5-cyclohexyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine in 200 ml of dimethylsulfoxide were added 28.1 g of 1-chloropinacolone, 28.8 g of potassium carbonate (powder), 1.15 g of potassium iodide and 1.35 g of tetrabutylammonium bromide. The mixture was stirred at room temperature for 4 hours. The reaction mixture was poured into ice water. The precipitate thus formed was collected by filtration with suction, washed with water and then dried, whereby 63.5 g of the title compound was obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06747022B2 |
| Quelldatensatz | uspto-grants-2004_06 |
| ORD ID | ord-71aa540e1d8e46a180281fff0427b79a |
| Quellennotiz | uspto-grants-2004_06 |