反应 #54159

ord-3f5c1017e42d4c01a4553abe59481e5b

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤After rinsing with nitrogen, 150 ml of acetone
  2. 2
    workup.ADDITIONwere added
  3. 3
    温度upon heating the reaction mixture for a longth of time
  4. 4
    温度under reflux
  5. 5
    其他After completion of the reaction
  6. 6
    萃取The organic layer was extracted three times with methylene chloride
  7. 7
    洗涤after which the combined extracts were washed
  8. 8
    其他dried
  9. 9
    其他After concentration of the organic layer by evaporation a product
  10. 10
    其他was obtained which
  11. 11
    其他crystallized out after a length of time (melting point 18°-20° C.)

实验过程

In a 500 ml-three-necked flask 4.8 g (0.01 mole) of the 2-chloro-4,6-dilauroxy-s-triazine prepared above, were mixed with 2.6 g (0.01 mole) of 2,6-diphenyl hydroquinone. After rinsing with nitrogen, 150 ml of acetone were added, followed by adding dropwise, with vigorous stilling, 0.4 g (0.01 mole) of NaOH dissolved in 7 ml of water, at 20° C. The solution then assumed an orange-yellow color, which largely disappeared upon heating the reaction mixture for a longth of time under reflux. After completion of the reaction, the contents of the flask were poured into 100 ml of ice water containing 2 ml of hydrochloric acid. The organic layer was extracted three times with methylene chloride, after which the combined extracts were washed and dried. After concentration of the organic layer by evaporation a product was obtained which crystallized out after a length of time (melting point 18°-20° C.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04147659uspto-grants-1979_04