HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Potassium Hydroxide → 4-(3,4-Dibromo-benzyl)-piperazine-1-carboxylic acid tert-butyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Edukt | 3,4-Dibromobenzaldehyde | HCID 622053 | — |
| Edukt | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(3,4-Dibromo-benzyl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 57880889 | 73,5% |
Reaktionsschritte
A solution of piperazine-1-carboxylic acid tert-butyl ester (3.5 g) and 3,4-dibromobenzaldehyde (5.0 g) in DCM (80 mL) was treated with NaB(OAc)3H (5.6 g). After 16 h, the resulting mixture was treated with 10% aq. KOH (80 mL). The aqueous phase was extracted with DCM (1×80 mL). The organic extracts were combined and dried (MgSO4). Most of the solvent was removed by concentration. Upon standing overnight, the resulting mixture produced crystals that were filtered and washed with DCM (1×5 mL), giving the title compound as a white crystalline solid (6.0 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08530476B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-59d2975d85a348a1993e3f7f99008638 |
| Quellennotiz | uspto-grants-2013_09 |