HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → HCID 21867318, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Sodium borohydride | HCID 4311764 | — |
| Edukt | ethyl 3-(5-amino-3-tert-butyl-1H-pyrazol-1-yl)benzoate | HCID 21867322 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | HCID 21867318 | HCID 21867318 | 87% |
Reaktionsschritte
To a solution of Intermediate 29a (1.00 g, 3.48 mmol) and Et3N (265 μL, 1.91 mmol) in EtOH (35 mL) was added NaBH4 (198 mg, 5.23 mmol) and the suspension stirred at RT for 1.5 h. NaBH4 (198 mg, 5.23 mmol) was added and the suspension stirred for a further 19 h. NaBH4 (1.31 g, 34.8 mmol) was added and the suspension stirred for a further 24 h, then diluted with water and extracted with DCM. The combined organics were dried and concentrated in vacuo. The residue was purified by FCC, using 0-10% [2M NH3 in MeOH] in DCM, to give the title compound as a white solid (740 mg, 87%). LCMS (Method 3): Rt 2.05 min, m/z 246 [MH+].
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09315503B2 |
| Quelldatensatz | uspto-grants-2016_04 |
| ORD ID | ord-43a0898a00d6435a80328f902108cfce |
| Quellennotiz | uspto-grants-2016_04 |