HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium Sulfate → (2R*,3R*,4R*,6S*)-3-(2,5-Dimethoxybenzyl)amino-2-diphenylmethyl-6-hydroxymethyl-1-azabicyclo[2.2.2]octane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium Sulfate | HCID 24436 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Edukt | (2R*,4S*,5S*,6S*)-N,N-dimethyl-5-(2,5-dimethoxybenzyl)amino-6-diphenylmethyl-1-azabicyclo[2.2.2]octane-2-carboxamide | HCID 70114647 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | (2R*,3R*,4R*,6S*)-3-(2,5-Dimethoxybenzyl)amino-2-diphenylmethyl-6-hydroxymethyl-1-azabicyclo[2.2.2]octane | HCID 54206645 | — |
Reaktionsschritte
Into a suspension of lithium aluminum hydride (LiAlH4) (92 mg, 2.4 mmole) in dry THF (10 ml) at 0° C. was added a solution of compound 35 (417 mg, 0.8 mmole) in dry THF (10 ml) and heated at reflux for 1 hour. Na2SO4 /10H2O was added to the reaction mixture and stirred for 30 minutes. After cooling, the solids were removed by filtration and washed with THF. The filtrate was evaporated, added excess 10% HCl/MeOH and concentrated down. The resulting oil was purified by recrystallization from MeOH-Ether. The white crystal was collected by filtration and dried in vacuo to give compound 41 2HCl salt (240 mg, 0.44 mmole, 55%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05716965 |
| Quelldatensatz | uspto-grants-1998_02 |
| ORD ID | ord-8ed5bc7461fe43b39f68ead5764f521a |
| Quellennotiz | uspto-grants-1998_02 |