HRID53945

反应详情

EQUATION

反应方程式

HRID 53945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a slurry consisting of 1,3-dihydro-1-[(phenylmethylene)amino]spiro[2H-indene-2,3'-[3H]indole]-2'(1'H)one (13.8 g), and absolute ethanol (300 ml) was added hydrazine hydrate (13.9 ml). The resulting mixture was heated at reflux for 3 hours, cooled to room temperature and the resulting precipitate removed by filtration. The mother liquor was concentrated and the resulting oil solidified upon addition of ethyl acetate-hexane. The resulting solid was recovered by filtration. Additional product was obtained from the mother liquor as above. Recrystallization from ethyl acetate afforded 1-amino- 1,3-dihydrospiro[2H-indene-2,3'-[3H]indol]-2'(1'H)one, m.p. 195°-197° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 3 hours
  3. customthe resulting precipitate removed by filtration
  4. concentrationThe mother liquor was concentrated
  5. additionthe resulting oil solidified upon addition of ethyl acetate-hexane
  6. filtrationThe resulting solid was recovered by filtration
  7. customAdditional product was obtained from the mother liquor as above
  8. customRecrystallization from ethyl acetate