HRID1068806
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 2.50 g (6.2 mmol) of 3-methyl-2-[5-(phthalimido)pentan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene in 50 ml of ethanol was added 928 mg (18.5 mmol) of hydrazinemonohydrate. The mixture was heated for two hours under reflux. After cooling, the resulting precipitates were collected by filtration and washed with ethanol. The filtrate and washing were combined and concentrated to give the residue. Water was added, extracted with methylene chloride, dried over anhydrous magnesium sulfate. The solvent was distilled off to afford 1.197 g of the desired compound (70.6%, a greenish brown solid).
WORKUP
后处理
- additionwas added 928 mg (18.5 mmol) of hydrazinemonohydrate
- temperatureThe mixture was heated for two hours
- temperatureunder reflux
- temperatureAfter cooling
- customthe resulting precipitates
- filtrationwere collected by filtration
- washwashed with ethanol
- washThe filtrate and washing
- concentrationconcentrated
- customto give the residue
- extractionextracted with methylene chloride
- dry with materialdried over anhydrous magnesium sulfate
- distillationThe solvent was distilled off