反应详情

A solution of spiro(cyclopentane-1,1'-indan)-3'-ylideneacetonitrile (10.5 g; 0.05 moles) in anhydrous ether (100 ml) is added dropwise under agitation to lithium aluminum hydride (2.5 g; 0.066 moles) suspended in ether (200 ml). After boiling for 3 hours the mixture is cooled to room temperature and the excess of hydride is decomposed by dropwise addition of a saturated sodium sulphate solution. The precipitate obtained is filtered off and washed with ether. The ether solutions are shaken with 2 N hydrochloric acid. The acid extracts are concentrated to a small volume in vacuum (bath temperature below 40° C.) and the amine hydrochloride is precipitated by treatment with conc. hydrochloric acid in the cooled. Yield 10.6 g (85%). Recrystallization from 2-propanol yields colourless crystals of mp. 190° C. identical with the product prepared according to example 3g.

1. customThe precipitate obtained
2. filtrationis filtered off
3. washwashed with ether
4. concentrationThe acid extracts are concentrated to a small volume in vacuum (bath temperature below 40° C.)
5. customthe amine hydrochloride is precipitated by treatment with conc. hydrochloric acid in the cooled
6. customRecrystallization from 2-propanol
7. customyields colourless crystals of mp. 190° C. identical with the product
8. customprepared