HRID1068798
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 suspension of 2.94 g (7.31 mmol) of 1,2-dihydro-3-methyl-1-[6-(phthalimido)hexan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one in 80 ml of ethanol was added 1.10 g (22.0 mmol) of hydrazine.monohydrate. The mixture was heated for 2 hours under reflux. After cooling, the resulting precipitates were filtered off. The filtrate was concentrated to give the residue, water was added, extracted with chloroform (three times). The extract was dried over anhydrous magnesium sulfate, then the solvent was distilled off to give 1.50 g of the desired compound (75.4%, pale yellow solid).
WORKUP
后处理
- temperatureThe mixture was heated for 2 hours
- temperatureunder reflux
- temperatureAfter cooling
- customthe resulting precipitates
- filtrationwere filtered off
- concentrationThe filtrate was concentrated
- customto give the residue, water
- additionwas added
- extractionextracted with chloroform (three times)
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off