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2,5-Hexanedione → alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]-N-(2,5-dimethyl-1-pyrrolyl)acetamide

HRID 1198911
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1198911
[CH2:1]([CH2:5][C:6](=O)[CH3:7])[C:2]([CH3:4])=O.[Cl:9][C:10]1[CH:21]=[C:20]([C:22]2[CH:23]([CH3:29])[NH:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:19]=[CH:18][C:11]=1[O:12][CH2:13][C:14]([NH:16][NH2:17])=[O:15]>C(O)(=O)C>[Cl:9][C:10]1[CH:21]=[C:20]([C:22]2[CH:23]([CH3:29])[NH:24][C:25](=[O:28])[NH:26][N:27]=2)[CH:19]=[CH:18][C:11]=1[O:12][CH2:13][C:14]([NH:16][N:17]1[C:6]([CH3:7])=[CH:5][CH:1]=[C:2]1[CH3:4])=[O:15]
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Komponenten

4

Edukt 2

HCID 80352,5-HexanedioneHCID 14370703alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide

Produkt 1

HCID 14370704alpha-[2-Chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]-N-(2,5-dimethyl-1-pyrrolyl)acetamideAusbeute 64 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

0.27 g of acetonylacetone was added to a solution of 0.5 g of α-[2-chloro-4-(2,3,4,5-tetrahydro-5-methyl-3-oxo-1,2,4-triazin-6-yl)phenoxy]acetohydrazide (prepared as described in Example 13) dissolved in 5 ml of acetic acid, and the mixture was heated at 70° C. for 4 hours. The acetic acid used as the solvent was removed by evaporation under reduced pressure, and the residue was mixed with water to precipitate crystals. These crystals were collected by filtration, washed with water and dried. The product was purified by column chromatography through silica gel (eluent: a 98:2 by volume mixture of methylene chloride and ethanol), followed by recrystallization from ethanol to give 0.4 g of the title compound melting at 189°-190° C.

Aufarbeitung

  1. customwas removed by evaporation under reduced pressure
  2. additionthe residue was mixed with water
  3. customto precipitate crystals
  4. filtrationThese crystals were collected by filtration
  5. washwashed with water
  6. customdried
  7. customThe product was purified by column chromatography through silica gel (eluent
  8. additiona 98:2 by volume mixture of methylene chloride and ethanol),
  9. customfollowed by recrystallization from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-6cce6df8eceb465ab733904b7383fd67
Quelldatensatz
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04898862

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