Ammonia → 3,4-Dichloro-5-isothiazolecarboxylic acid amide

HRID 478133Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 478133
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8](Cl)=[O:9])[S:4][N:3]=1.[NH3:11]>O>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8]([NH2:11])=[O:9])[S:4][N:3]=1

Komponenten

4

Edukt 2

HCID 222Ammonia2×HCID 109768863,4-Dichloro-5-isothiazolecarbonyl chloride

Produkt 1

HCID 113330673,4-Dichloro-5-isothiazolecarboxylic acid amideAusbeute 82 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

At 0 to 10° C., 50.1 g (0.2 mol) of 3,4-dichloro-isothiazole-5-carbonyl chloride are added dropwise with stirring over a period of 30 minutes to 82 g (1.2 mol) of concentrated ammonia. After the addition, another 41 g (0.6 mol) of concentrated ammonia are added and the mixture is diluted with 70 ml of water. The mixture is allowed to warm to room temperature and stirred at this temperature for 45 minutes. The resulting precipitate is filtered off with suction, washed successive with water and petroleum ether and dried. In this manner, 32.3 g (81.8% of theory) of 3,4-dichloro-isothiazole-5-carboxamide are obtained in the form of a solid of melting point 156 to 158° C.

Aufarbeitung

  1. additionAfter the addition
  2. filtrationThe resulting precipitate is filtered off with suction
  3. washwashed successive with water and petroleum ether
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3a75e08db54948c8a118203cb47f7069
Quelldatensatz
uspto-grants-2003_11
Patentnummer
US06642181B2

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