Reaktion #1946560

ord-45bf06e15d644313a0a134eda93238f9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewas prepared, to which
  2. 2
    Temperaturheated on a steam bath for 23 hrs
  3. 3
    Temperaturcooled
  4. 4
    ExtraktionThe mixture was extracted with methylene chloride
  5. 5
    Waschenthe extracts were washed with water
  6. 6
    Trocknendried over magnesium sulfate
  7. 7
    Einengenconcentrated
  8. 8
    Sonstigeto crystallize on standing
  9. 9
    Sonstigewas used without further purification

Vorschrift

A mixture of 114.95 g (356.5 mmol) of N,N-di-n-butyl-N′-(3-methoxybenzoyl)thiourea (compound 1-24), 31.37 g (784.2 mmol) of sodium hydroxide, and 350 ml of water was prepared, to which was added 40.42 g (427.8 mmol) of chloroacetic acid. The mixture was stirred and heated on a steam bath for 23 hrs, then cooled. The mixture was extracted with methylene chloride, and the extracts were washed with water, dried over magnesium sulfate, and concentrated. The oily residue began to crystallize on standing. The yield of thiazole was 100.8 g and was used without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06528223B1uspto-grants-2003_03