HRID53945
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting mixture was heated
- temperatureat reflux for 3 hours
- customthe resulting precipitate removed by filtration
- concentrationThe mother liquor was concentrated
- additionthe resulting oil solidified upon addition of ethyl acetate-hexane
- filtrationThe resulting solid was recovered by filtration
- customAdditional product was obtained from the mother liquor as above
- customRecrystallization from ethyl acetate