반응 #1946560

ord-45bf06e15d644313a0a134eda93238f9

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was prepared, to which
  2. 2
    온도heated on a steam bath for 23 hrs
  3. 3
    온도cooled
  4. 4
    추출The mixture was extracted with methylene chloride
  5. 5
    세척the extracts were washed with water
  6. 6
    건조dried over magnesium sulfate
  7. 7
    농축concentrated
  8. 8
    기타to crystallize on standing
  9. 9
    기타was used without further purification

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06528223B1uspto-grants-2003_03