Ethyl 2-chloroacetoacetate → HCID 178432410, Verbindung

HRID 477222

Reaktionsgleichung

Reaktionsgleichung von HRID 477222
[NH2:1][C:2]1[N:6]=[C:5]([S:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[NH:4][N:3]=1.[Cl:15][CH:16]([C:22]([CH3:24])=O)[C:17](OCC)=[O:18]>C(O)(=O)C>[CH2:8]([S:7][C:5]1[N:6]=[C:2]2[N:1]=[C:22]([CH3:24])[C:16]([Cl:15])=[C:17]([OH:18])[N:3]2[N:4]=1)[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

Komponenten

4

Edukt 2

HCID 11858Ethyl 2-chloroacetoacetateHCID 178509291HCID 178509291, Verbindung

Produkt 1

HCID 178432410HCID 178432410, VerbindungAusbeute 60 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of 16 g (77 mmol) of 3-amino-5-benzylthio-1,2,4-triazole and 10.6 g (77 mmol) of ethyl 2-chloroacetoacetate in 150 ml of glacial acetic acid was heated at 100° C. for 17 hours. Upon cooling to room temperature the solid which separated was collected by filtration. The filtrate was diluted with ice water to separate an additional quantity of solid. The solids were combined and dried to yield 14.0 g (60% of the desired product as a solid, m.p. 258°-260° C. IR and 1H NMR were in agreement with the assigned structure.

Aufarbeitung

  1. customseparated
  2. filtrationwas collected by filtration
  3. additionThe filtrate was diluted with ice water
  4. customto separate an additional quantity of solid
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-11643bfd920c48288a6c4f28df5dc2d5
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04886883

Verknüpfte Notizen

Wird geladen…