反応 #55253

ord-b7218be49b3d482993418ba5ee590b49

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared
  2. 2
    その他is kept at 0°-5° C. by means of external cooling
  3. 3
    workup.ADDITIONAfter the addition
  4. 4
    ろ過Filtering
  5. 5
    その他recrystallisation of the product from ethyl acetate/hexane

実験手順

62.4 g of 2,2,6,6-tetramethyl-4-amino-piperidine in 200 ml of acetone and, at the same time, 42.4 g of sodium carbonate dissolved in 100 ml of water are added to a finely dispersed suspension of cyanuric chloride, prepared by adding 36.9 g of the latter in 200 ml of boiling acetone to 400 ml of ice water. The temperature is kept at 0°-5° C. by means of external cooling. After the addition is complete, the reaction mixture is allowed slowly to warm to room temperature and is stirred at this temperature for 3 hours. Filtering and recrystallisation of the product from ethyl acetate/hexane gives 46.3 g of a white crystalline product, melting point 270° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04151356uspto-grants-1979_04