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Ammonium Chloride → 5-(5-Isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-(4-methoxy-phenyl)-2,4-dihydro-[1,2,4]triazol-3-thione

HRID 1947185
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1947185
COC1C=CC([N:9]([C:14](=O)[C:15]2[CH:20]=[C:19]([CH:21]([CH3:23])[CH3:22])[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]=2[O:28][CH2:29][O:30][CH3:31])[NH:10][C:11]([NH2:13])=[S:12])=CC=1.[Cl-].[NH4+]>[OH-].[Na+]>[CH:21]([C:19]1[C:18]([O:24][CH2:25][O:26][CH3:27])=[CH:17][C:16]([O:28][CH2:29][O:30][CH3:31])=[C:15]([C:14]2[N:13]([C:15]3[CH:20]=[CH:19][C:18]([O:24][CH3:25])=[CH:17][CH:16]=3)[C:11](=[S:12])[NH:10][N:9]=2)[CH:20]=1)([CH3:23])[CH3:22]
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Komponenten

4

Edukt 2

HCID 25517Ammonium ChlorideHCID 866243104-Methoxyphenyl-1-[5-isopropyl-2,4-bis(methoxymethoxy)-benzoyl]thiosemicarbazide

Produkt 1

HCID 598298385-(5-Isopropyl-2,4-bis-methoxymethoxy-phenyl)-4-(4-methoxy-phenyl)-2,4-dihydro-[1,2,4]triazol-3-thioneAusbeute 171,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

4-methoxyphenyl-1-[5-isopropyl-2,4-bis(methoxymethoxy)-benzoyl]thiosemicarbazide (F53-03: 24.9 g, 53.7 mmol) and 5% aqueous sodium hydroxide (500 mL) were placed in a 1 L eggplant shaped flask and heated under reflux for 1 hour. After completing the reaction, the reaction mixture was neutralized with saturated aqueous ammonium chloride, and the solids deposited were collected by filtration, washed with distilled water and then dried under reduced pressure. The crude product thus obtained was purified by suspending in ethyl acetate/hexane and concentrating under reduced pressure to obtain the title compound (F53-04:20.5 g, 85.4%).

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 1 hour
  3. customthe reaction
  4. filtrationthe solids deposited were collected by filtration
  5. washwashed with distilled water
  6. customdried under reduced pressure
  7. customThe crude product thus obtained
  8. customwas purified
  9. concentrationconcentrating under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-8640c80a99af45dcaafb9806b37f2c0b
Quelldatensatz
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08399464B2

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