Hydrochloric Acid → HCID 14500702, Verbindung

HRID 2350885Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2350885
[CH:1]1([NH:7][C:8](=S)[NH:9][NH2:10])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[Cl:12][CH:13]([C:19]([CH3:21])=O)[C:14]([O:16][CH2:17][CH3:18])=[O:15].Cl>C(O)C>[ClH:12].[CH:1]1([NH:7][C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:19]([CH3:21])[NH:10][N:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 11858Ethyl 2-chloroacetoacetateHCID 722813Hydrazinecarbothioamide, N-cyclohexyl-

Produkt 1

HCID 14500702HCID 14500702, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 34.7 g (0.2 mole) of 4-cyclohexyl-3-thiosemicarbazide and 32.9 g (0.2 mole) of ethyl 2-chloroacetoacetate in 350 mL of absolute ethanol was stirred under nitrogen atmosphere at ambient temperature for 2 hr, treated with 100 mL of 2N ethanolic hydrogen chloride and heated at reflux for 2 hr. The hot reaction mixture was filtered to remove an amorphous solid. The product persistently crystallized in the filter. The product was recrystallized from acetone and recovered by decating off hot acetone solvent and washing the residue with cold acetone to give 27 g of large, off-white crystals, mp 178-182° C.

Aufarbeitung

  1. temperatureheated
  2. temperatureat reflux for 2 hr
  3. filtrationThe hot reaction mixture was filtered
  4. customto remove an amorphous solid
  5. customThe product persistently crystallized in the filter
  6. customThe product was recrystallized from acetone
  7. customrecovered
  8. washwashing the residue with cold acetone
  9. customto give 27 g of large, off-white crystals, mp 178-182° C.

Quellen und Nachweise

ORD-Eintrag
ord-5d4935ef508d4b9cb379f60c4e3f41f1
Quelldatensatz
uspto-grants-1989_10
Patentnummer
US04871737

Notizen zur Reaktion

Wird geladen…