反应详情

A solution of 1.36 g (5.0 mmol) 2-methyl-7-(phenylmethy)-2,7-diazaspiro[4.4]nonane-1,3,8-trione in 50 ml tetrahydrofuran was added dropwise to a suspension of 0.95 g (25 mmol) lithium aluminum hydride in 30 ml tetrahydrofuran. Ihe mixture was stirred overnight at room temperature, refluxed one hour, cooled, and treated dropwise with 0.95 ml water, 0.95 ml 15% sodium hydroxide solution and 2.8 ml water. After removal of the inorganic solids by filtration, the filtrate was concentrated in vacuo to give a syrup which was dissolved in isopropanol and treated with excess 6N hydrogen chloride in isopropanol. Crystallization afforded 0.97 g of 2-methyl-7-(phenylmethyl)-2,7-diazaspiro[4.4]nonane dihydrochloride, mp 233-234° C.

1. temperaturerefluxed one hour
2. temperaturecooled
3. customAfter removal of the inorganic solids
4. filtrationby filtration
5. concentrationthe filtrate was concentrated in vacuo
6. customto give a syrup which
7. customCrystallization