反応 #318559

ord-4e26d05449f846529a1c30fbcf8ff566

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度is heated
  2. 2
    温度to reflux of the dioxon
  3. 3
    その他The product expected crystallizes
  4. 4
    洗浄washing with water
  5. 5
    その他drying
  6. 6
    温度by heating under vacuum
  7. 7
    その他the product is recrystallized from acetonitrile

実験手順

The mixture consisting of 0.1 mole (22.6 g) of 2,4,6-trichloronitrobenzene, 0.6 mole (63 g) of 2-(β-aminoethoxy)ethanol and 20 ml of dioxan is heated to reflux of the dioxon. After 4 hours, the reaction mixture is poured onto to 200 g of ice. The product expected crystallizes on acidifying with concentrated hydrochloric acid. After draining, washing with water and drying by heating under vacuum, the product is recrystallized from acetonitrile and then from toluene. It melts at 83° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04845293uspto-grants-1989_07