反応 #4856

ord-0f00b2a48ac44f1f81b28c45b15724f2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONhas been added
  2. 2
    温度Heating
  3. 3
    温度is maintained for 20 minutes
  4. 4
    workup.ADDITIONafter the addition
  5. 5
    温度When the mixture is cooled

実験手順

To a suspension of 0.119 mole (27 g) of 2-(2-amino-3,5-dinitrophenyl)ethanol obtained in Example 1 in 67.5 ml of isopropanol to which an equal volume of water has been added, a solutionof 38.4 g of sodium sulphide nonahydrate and 5.4 g of sulphur in 10 ml of water is added dropwise at 60°-65° C. Heating is maintained for 20 minutes after the addition is complete. When the mixture is cooled, a precipitate of the expected product is obtained, and this is drained, made into a paste in water and then recrystallized from 96° strength alcohol. It melts at 172° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04727192uspto-grants-1988_02