Potassium thiocyanate → 4-Tert-butyl-1,3-dihydroimidazole-2-thione

HRID 1679671Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1679671
Cl.[NH2:2][CH2:3][C:4](=O)[C:5]([CH3:8])([CH3:7])[CH3:6].[S-:10][C:11]#[N:12].[K+]>O>[C:5]([C:4]1[N:12]=[C:11]([SH:10])[NH:2][CH:3]=1)([CH3:8])([CH3:7])[CH3:6]

Komponenten

4

Edukt 2

HCID 516872Potassium thiocyanateHCID 221479671-Amino-3,3-dimethylbutan-2-one hydrochloride

Produkt 1

HCID 1784413604-Tert-butyl-1,3-dihydroimidazole-2-thione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

35.2 g. 1-Amino-3,3-dimethylbutan-2-one hydrochloride and 30 g. potassium thiocyanate in 50 ml. water was warmed on the steam bath for two hours. After cooling, the solid formed was collected, washed with water, dried and recrystallised from industrial methylated spirit to give 4-tert.butylimidazole-2-thiol, melting point 232°-234° C. A solution/suspension of this in industrial methylated spirit was added to a solution of 4.5 g. sodium hydroxide in 100 ml. water. 17.6 g. Ethyl iodide was added forming a lower layer and the mixture was shaken for two minutes whilst the ethyl iodide reacted and dispersed. After 20 minutes the alkali was neutralised by passing in carbon dioxide and the methylated spirit removed by evaporation. The solid was collected, washed with water, dried and on recrystallisation from toluene gave 2-ethylthio-4-tert.butylimidazole, melting point 116.5°-120° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe solid formed
  3. customwas collected
  4. washwashed with water
  5. customdried
  6. customrecrystallised from industrial methylated spirit

Quellen und Nachweise

ORD-Eintrag
ord-845a8f7acb8a4e16998abbb3cbdabb90
Quelldatensatz
uspto-grants-1978_03
Patentnummer
US04081540

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