Methane → HCID 131712839, Verbindung

HRID 1702847

Reaktionsgleichung

Reaktionsgleichung von HRID 1702847
[CH2:1]([O:3][C:4]([C:6]1[C:7]([Cl:16])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2].C.[CH2:18]([NH:22][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[S:24])[CH2:19][CH2:20][CH3:21]>CC(C)=O>[ClH:16].[CH2:1]([O:3][C:4]([C:6]1[C:7]([S:24][C:23]([NH:25][CH2:26][CH2:27][CH2:28][CH3:29])=[N:22][CH2:18][CH2:19][CH2:20][CH3:21])=[N:8][C:9]2[C:14]([N:15]=1)=[CH:13][CH:12]=[CH:11][CH:10]=2)=[O:5])[CH3:2]

Komponenten

5

Edukt 3

HCID 297Methane2×HCID 2723622N,N'-DibutylthioureaHCID 12283436Ethyl 3-Chloroquinoxaline-2-carboxylate

Produkt 1

HCID 131712839HCID 131712839, VerbindungAusbeute 47,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Versuchsvorschrift

2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (7.10 g., 0.03 mole) was dissolved in 125 ml. of acetone treated with Norit and filtered. The filtrate was added to 5.650 g. (0.03 mole) of 1,3-di-n-butylthiourea in 100 ml. of acetone. The solution was stirred at reflux under a nitrogen atmosphere for 6 hours, allowed to cool to room temperature, and stirred an additional 17 hours. The red solution was treated with Norit, filtered, and concentrated to a volume of 100 ml. The yellow solid that crystallized out was collected by filtration, washed and dried to give the 6.05 g. (47.5% yield) of product, m.p. 138°-139° C. (dec.).

Aufarbeitung

  1. filtrationfiltered
  2. additionThe filtrate was added to 5.650 g
  3. temperatureat reflux under a nitrogen atmosphere for 6 hours
  4. stirringstirred an additional 17 hours
  5. filtrationfiltered
  6. concentrationconcentrated to a volume of 100 ml
  7. customThe yellow solid that crystallized out
  8. filtrationwas collected by filtration
  9. washwashed
  10. customdried
  11. customto give the 6.05 g

Quellen und Nachweise

ORD-Eintrag
ord-f825206e528846759b677540039b12f1
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04349674

Verknüpfte Notizen

Wird geladen…