تفاعل #1946560

ord-45bf06e15d644313a0a134eda93238f9

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىwas prepared, to which
  2. 2
    درجة الحرارةheated on a steam bath for 23 hrs
  3. 3
    درجة الحرارةcooled
  4. 4
    استخلاصThe mixture was extracted with methylene chloride
  5. 5
    غسيلthe extracts were washed with water
  6. 6
    تجفيفdried over magnesium sulfate
  7. 7
    تركيزconcentrated
  8. 8
    أخرىto crystallize on standing
  9. 9
    أخرىwas used without further purification

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06528223B1uspto-grants-2003_03