Sodium sulfate decahydrate → 4-Amino-3,5-dichlorobenzylamine

HRID 1432060

Reaktionsgleichung

Reaktionsgleichung von HRID 1432060
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([Cl:17])[C:15]=1[NH2:16])[C:11]#[N:12].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[Cl:7][C:8]1[CH:9]=[C:10]([CH:13]=[C:14]([Cl:17])[C:15]=1[NH2:16])[CH2:11][NH2:12]

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 5227064-Amino-3,5-dichlorobenzonitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 189757634-Amino-3,5-dichlorobenzylamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

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 3.65 (s, 2H), 7.2 (s, 2H).

Aufarbeitung

  1. stirringstirred for 30 min
  2. filtrationThe solid was filtered off
  3. washwashed with THF for three times
  4. customThe solvent was removed by rotovap and residue
  5. customwas purified by column with Methanol/DCM (3:7) as the eluant

Quellen und Nachweise

ORD-Eintrag
ord-59322ad98b934b5794322c1317f477a9
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07612069B2

Verknüpfte Notizen

Wird geladen…