HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → (3-(tert-Butoxycarbonyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yl)boronic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Ammonium Acetate | HCID 517165 | — |
| Edukt | Sodium periodate | HCID 23667635 | — |
| Edukt | tert-Butyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-benzo[d]azepine-3-carboxylate | HCID 57505869 | — |
| Lösungsmittel | Acetone | HCID 180 | — |
| Produkt | (3-(tert-Butoxycarbonyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yl)boronic acid | HCID 57440296 | 84,9% |
Reaktionsschritte
1,1-Dimethylethyl 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (E264, Step 1) (1.60 g, 4.29 mmol) was dissolved in acetone (25 ml), treated with sodium periodate (2.75 g, 12.9 mmol), ammonium acetate (0.73 g, 9.44 mmol) and water (25 ml) and the resulting mixture was stirred for 18 hours at room temperature. The acetone was removed by evaporation in vacuo and the remaining water layer was extracted with ethyl acetate and dichloromethane. The organic layers were combined, dried under magnesium sulfate and evaporated in vacuo to give the title compound (1.06 g); MS (ES+) m/e 192 [(M+H)—CO2tBu]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07704994B2 |
| Quelldatensatz | uspto-grants-2010_04 |
| ORD ID | ord-4349a7eb67244611accb8753fdc2a560 |
| Quellennotiz | uspto-grants-2010_04 |