反応 #54324

ord-39344a9a84f247b1a5f14467327c0645

反応方程式

[K]
potassium
O=C1C=CC(=O)O1
maleic anhydride
Oc1ccc(Nc2ccccc2)cc1
4-anilinophenol
Oc1ccc(Nc2ccccc2)cc1
4-anilinophenol
Cl
hydrochloric acid
[K]
potassium
O=C(O)/C=C\C(=O)Oc1ccc(Nc2ccccc2)cc1
4-Anilinophenyl hydrogen maleate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was prepared
  2. 2
    その他prepared
  3. 3
    その他The organic layer was separated by extraction with benzene
  4. 4
    洗浄The extract was washed twice with water
  5. 5
    その他to evaporate
  6. 6
    その他The residue was recrystallized twice from benzene yielding 1.3 grams of product which melted at 139°-142° C.

実験手順

4-Anilinophenyl hydrogen maleate was prepared by adding 10 grams of maleic anhydride to a solution of the potassium salt of 4-anilinophenol which was prepared by dissolving 18.5 grams of 4-anilinophenol in a solution of potassium tert.butoxide prepared by reacting 3.9 grams of potassium with 75 milliliters of tert.butyl alcohol. The reaction mixture was stirred for two hours at 65°-70° C. and was then poured into a solution of 12 milliliters of concentrated hydrochloric acid in 138 milliliters of water. The organic layer was separated by extraction with benzene. The extract was washed twice with water and then allowed to evaporate. The residue was recrystallized twice from benzene yielding 1.3 grams of product which melted at 139°-142° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04147880uspto-grants-1979_04