HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methanesulfonic Acid → 5-(N,N-Diethylaminomethyl)-3-(2,5-dimethoxybenzylamino)-2-diphenylmethyl-1-azabicyclo[2.2.2]octane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methanesulfonic Acid | HCID 6395 | — |
| Edukt | Sodium Sulfate | HCID 24436 | — |
| Edukt | N,N-Diethyl-5-(2,5-dimethoxy benzylamino)-6-diphenylmethyl-1-azabicyclo[2.2.2]octane-3-carboxamide | HCID 10165826 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 5-(N,N-Diethylaminomethyl)-3-(2,5-dimethoxybenzylamino)-2-diphenylmethyl-1-azabicyclo[2.2.2]octane | HCID 70115721 | 57% |
Reaktionsschritte
A solution of 19 (300 mg, 0.55 mmole) in dry THF (2 ml) was added to a suspension of LiAIH4 (105 mg, 2.75 mmole) in 5 ml of dry THF at 5° C. and stirred at room temperature for 1 hour. Na2SO4 /10H2O (2 g) was added to the reaction mixture and stirred for 15 hours at room temperature. The suspension was filtrated, and the solids were washed with dry THF. The filtrate was concentrated under reduced pressure. The resulting oil was dissolved in 2 ml of acetone, and CH3SO3H (159 mg, 1.65 mmole) was added to the solution of the crude oil in acetone (2 ml). The resulting precipitate was collected by filtration and dried in vacuo to give 20 (254 mg, 0.31 mmole, 57%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05852038 |
| Quelldatensatz | uspto-grants-1998_12 |
| ORD ID | ord-fdc3a328f762429494463eeedb04a933 |
| Quellennotiz | uspto-grants-1998_12 |