反応 #554616

ord-76e27b87190741a5b724e9b4411db060

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他In a reaction vessel equipped with an agitator
  2. 2
    その他the mixture was reacted at the same temperature for one hour
  3. 3
    その他further reacted for one hour
  4. 4
    抽出extracted with ethyl acetate
  5. 5
    洗浄The organic layer was washed with water
  6. 6
    その他separated
  7. 7
    乾燥it was then dried with magnesium sulfate
  8. 8
    濃縮subjected to vacuum concentration
  9. 9
    その他Thus, the objective product was obtained with the yield of 2.38 g

実験手順

In a reaction vessel equipped with an agitator, thermometer and a cooling pipe, 2.1 g of p-tolyl-bis(6-methoxy-2-naphthyl)amine and 50 mL of methylene chloride were placed. While the vessel was being cooled with ice, 12 mL of a 1M methylene chloride solution of boron tribromide was delivered by drops into the vessel, and the mixture was reacted at the same temperature for one hour. The temperature was raised to a room temperature and further reacted for one hour. Then, the reacted solution was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and separated, and it was then dried with magnesium sulfate and subjected to vacuum concentration. Thus, the objective product was obtained with the yield of 2.38 g.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08623577B2uspto-grants-2014_01