反応 #1946560

ord-45bf06e15d644313a0a134eda93238f9

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was prepared, to which
  2. 2
    温度heated on a steam bath for 23 hrs
  3. 3
    温度cooled
  4. 4
    抽出The mixture was extracted with methylene chloride
  5. 5
    洗浄the extracts were washed with water
  6. 6
    乾燥dried over magnesium sulfate
  7. 7
    濃縮concentrated
  8. 8
    その他to crystallize on standing
  9. 9
    その他was used without further purification

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06528223B1uspto-grants-2003_03