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

HRID 133785

Reaktionsgleichung

Reaktionsgleichung von HRID 133785
[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 B (2): 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 one portion and the resulting mixture was stirred for 3 h. Sodium sulfate decahydrate (1 g, 3.2 mmol) was added in one portion and the mixture was stirred for 30 min. The solid was filtered off and the filtrate was concentrated. The residue was purified by HPLC to give 4-acetamido-3,5-dichloro-benzylamine (35 mg, 30%). 1H NMR (500 MHz, CD3OD): δ 7.46 (s, 2 H), 3.78 (s, 2H), 2.18 (s, 3 H).

Aufarbeitung

  1. stirringthe mixture was stirred for 30 min
  2. filtrationThe solid was filtered off
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by HPLC

Quellen und Nachweise

ORD-Eintrag
ord-cc504b15272a48c7a93affceaa977dc8
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07390925B2

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