Sodium sulfate decahydrate → N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamide

HRID 1432074

Reaktionsgleichung

Reaktionsgleichung von HRID 1432074
[C:1]([NH:4][C:5]1[C:12]([Cl:13])=[CH:11][C:8]([C:9]#[N:10])=[CH:7][C:6]=1[Cl:14])(=[O:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[C:1]([NH:4][C:5]1[C:6]([Cl:14])=[CH:7][C:8]([CH2:9][NH2:10])=[CH:11][C:12]=1[Cl:13])(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 62649Sodium sulfate decahydrateHCID 2735977N-(2,6-dichloro-4-cyanophenyl)acetamideHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 58962993N-(4-(aminomethyl)-2,6-dichlorophenyl)acetamideAusbeute 30 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Step AT2. To a solution of 4-acetamido-3,5-dichloro-benzonitrile (114 mg, 0.5 mmol) in 5 mL of THF was added lithium aluminum hydride (120 mg, 3.2 mmol) in portion and the resulting mixture was stirred for 3 hours. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in portion and the mixture was stirred for 30 minutes. The solid was filtered off and the filtration was concentrated. Residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%).

Aufarbeitung

  1. stirringthe mixture was stirred for 30 minutes
  2. filtrationThe solid was filtered off
  3. filtrationthe filtration
  4. concentrationwas concentrated
  5. customResidue was purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-27e4930584df49deaf113f207d70c4b4
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07612069B2

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