HRID1600879

反应详情

EQUATION

反应方程式

HRID 1600879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 200 ml of t-amyl alcohol were poured 12.9 g of 97% oxindole, 20.0 g of 4,4'-diaminobenzophenone, and 26.43 g of potassium-t-butoxide. By use of a Molecular Sieves 4A tower which served as a dehydrator, the resultant mixture was refluxed with heat for 12 hours. Thereafter, the reaction mixture was cooled. An aqueous solution prepared by diluting 25 g of 35% HCl with 200 g water was added. The resultant mixture was stirred for 1.5 hours while being cooled with ice, and yellow crystals that precipitated were collected by filtration. The resultant crude product was washed with acetone, to thereby obtain 4.6 g (yield 15%) of the title compound in the form of yellow crystals. The melting point and elementary analysis data are shown in Table 15, and NMR and MS spectrum data are shown in Table 16.

WORKUP

后处理

  1. temperaturewith heat for 12 hours
  2. temperatureThereafter, the reaction mixture was cooled
  3. customAn aqueous solution prepared
  4. additionwas added
  5. temperaturewhile being cooled with ice, and yellow crystals that
  6. customprecipitated
  7. filtrationwere collected by filtration
  8. washThe resultant crude product was washed with acetone