HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium sulfate decahydrate → 4-Amino-3,5-dichlorobenzylamine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium sulfate decahydrate | HCID 62649 | — |
| Edukt | 4-Amino-3,5-dichlorobenzonitrile | HCID 522706 | — |
| Edukt | Aluminium lithium hydride | HCID 21226445 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 4-Amino-3,5-dichlorobenzylamine | HCID 18975763 | — |
Reaktionsschritte
To lithium aluminum hydride (0.57 g, 15 mmol) in dry THF (20 mL) was added dropwise 3,5-dichloro-4-aminobenzonitrile (1.87 g, 10 mmol) in THF (30 mL). The mixture was stirred at RT for 2 hours. Then, sodium sulfate decahydrate (4.83 g, 15 mmol) was added and stirred for 30 min. The solid was filtered off and washed with THF for three times. The solvent was removed by rotovap and residue was purified by column with Methanol/DCM (3:7) as the eluant. 3,5-dichloro-4-aminobenzylamine was obtained as an off-white solid (1.5 g, 80%). 1H NMR (300 MHz, CD3OD): δ 7.2 (s, 2H), 3.65 (s, 2H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07732434B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-ed8d7956d0384a1687ead6d120fd7703 |
| Quellennotiz | uspto-grants-2010_06 |