HRID66622

反应详情

EQUATION

反应方程式

HRID 66622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 5.6 g. of N-decyl-3-phenyl-3-(4-nitrophenyl)propenamide in 80 ml. of glacial acetic acid, at 85° C., was added, portionwise, during 20 minutes, 3.85 g. of iron powder. The reaction was exothermic and the temperature was between 85° and 90° C. during the addition. After the addition, the reaction mixture was filtered and the solids were washed with further hot acetic acid. The combined acetic acid solutions were evaporated in vacuo and the residue was partitioned between ethyl acetate and water. The ethyl acetate layer was removed, washed with water, and dried. Evaporation in vacuo gave an oil which solidified. The solid was recrystallized from isopropyl ether, giving 2.3 g. of the title compound, m.p. 90°-100° C.

WORKUP

后处理

  1. additionthe temperature was between 85° and 90° C. during the addition
  2. additionAfter the addition
  3. filtrationthe reaction mixture was filtered
  4. washthe solids were washed with further hot acetic acid
  5. customThe combined acetic acid solutions were evaporated in vacuo
  6. customthe residue was partitioned between ethyl acetate and water
  7. customThe ethyl acetate layer was removed
  8. washwashed with water
  9. customdried
  10. customEvaporation in vacuo
  11. customgave an oil which
  12. customThe solid was recrystallized from isopropyl ether
  13. customgiving 2.3 g