Triethylamine → HCID 18546092, Verbindung

HRID 1267214Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1267214
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8](Cl)=[O:9])[S:4][N:3]=1.[NH2:11][CH:12]([CH:15]([CH3:17])[CH3:16])[C:13]#[N:14].C(N(CC)CC)C>ClCCl>[C:13]([CH:12]([NH:11][C:8]([C:5]1[S:4][N:3]=[C:2]([Cl:1])[C:6]=1[Cl:7])=[O:9])[CH:15]([CH3:17])[CH3:16])#[N:14]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 104191372-Amino-3-methylbutyronitrileHCID 109768863,4-Dichloro-5-isothiazolecarbonyl chloride

Produkt 1

HCID 18546092HCID 18546092, VerbindungAusbeute 55,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

A solution of 3,4-dichloro-5-isothiazolecarboxylic acid chloride (2.1 g) in dichloro-methane (5 ml) was added drop by drop to a solution of 2-amino-3-methyl-butyronitrile (1.2 g) and triethylamine (1.5 g) in dichloromethane (10 ml) under ice cooling. After the addition was completed, the temperature was brought to room temperature, and the mixture was stirred for further 4 hours. The reaction mixture was then washed with water and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the remaining residue was purified by silica gel column chromatography (eluent: chloroformn) to obtain N-(1-cyano-2-methyl-propyl)-3,4-dichloro-5-isothiazolecarboxamide (1.5 g) (mp 120-121° C.).

Aufarbeitung

  1. additionAfter the addition
  2. customwas brought to room temperature
  3. washThe reaction mixture was then washed with water
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe remaining residue was purified by silica gel column chromatography (eluent: chloroformn)

Quellen und Nachweise

ORD-Eintrag
ord-dfb2a1fd6a8d4420a8e434bf90b4f0de
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06552056B2

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