Diethyl Ether → 2-[(3-chloro-4-methyl-2-thienyl)carbonyl]-N-isobutylhydrazinecarboxamide

HRID 660912

Reaktionsgleichung

Reaktionsgleichung von HRID 660912
[Cl:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([NH:10][NH2:11])=[O:9].[CH2:12]([N:16]=[C:17]=[O:18])[CH:13]([CH3:15])[CH3:14].C(OCC)C>C1COCC1>[Cl:1][C:2]1[C:6]([CH3:7])=[CH:5][S:4][C:3]=1[C:8]([NH:10][NH:11][C:17]([NH:16][CH2:12][CH:13]([CH3:15])[CH3:14])=[O:18])=[O:9]

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 612812-Methylpropyl isocyanateHCID 27775683-Chloro-4-methyl-2-thiophenecarboxylic acid hydrazide

Produkt 1

HCID 580122082-[(3-chloro-4-methyl-2-thienyl)carbonyl]-N-isobutylhydrazinecarboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

1.00 g (5.25 mmol) of 3-chloro-4-methylthien-2-ylcarboxylic acid hydrazide are placed in 10 ml THF at room temperature. 520 mg (5.25 mmol) of isobutyl isocyanate, dissolved in 2 ml THF, are rapidly added dropwise with stirring. The mixture is further stirred overnight at room temperature. For the workup, the reaction mixture is treated with 10 ml diethyl ether, cooled in the water/ice-bath to about 0° C., and the resulting precipitate recovered by filtration, washed with diethyl ether and dried in vacuo. 1.29 g (85% of theory) of the target compound are thus obtained.

Aufarbeitung

  1. additionare rapidly added dropwise
  2. filtrationthe resulting precipitate recovered by filtration
  3. washwashed with diethyl ether
  4. customdried in vacuo
  5. custom1.29 g (85% of theory) of the target compound are thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-b86eac4de23e4e6ea08a2140093682a2
Quelldatensatz
uspto-grants-2011_12
Patentnummer
US08084481B2

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