Thioacetamide → HCID 66673711, Verbindung

HRID 421835Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 421835
[C:1]([NH2:4])(=[S:3])[CH3:2].Br[CH2:6][C:7]([N:9]1[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1)=O>C(O)C>[CH3:2][C:1]1[S:3][CH:6]=[C:7]([N:9]2[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[N:4]=1

Komponenten

4

Edukt 2

HCID 2723949ThioacetamideHCID 15829155tert-Butyl 4-(bromoacetyl)piperazine-1-carboxylate

Produkt 1

HCID 66673711HCID 66673711, VerbindungAusbeute 2,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Thioacetamide (120 mg) was added to an ethanol (6 mL) solution of tert-butyl 4-(bromoacetyl)piperazinecarboxylate (340 mg) obtained in the above 1), and heated under reflux for 3 hours. The reaction liquid was restored to room temperature, then the solvent was evaporated away under reduced pressure, and the resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3) to obtain 7 mg of the entitled compound.

Aufarbeitung

  1. customobtained in the above 1), and
  2. temperatureheated
  3. temperatureunder reflux for 3 hours
  4. customThe reaction liquid
  5. customwas restored to room temperature
  6. customthe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified through silica gel column chromatography (hexane/ethyl acetate=7/3)

Quellen und Nachweise

ORD-Eintrag
ord-5049bb1cc5e24c538645131813f4771e
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08101618B2

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