N,N,N',N'-Tetramethylethylenediamine → HCID 53867368, compound

Participants

Reaction Steps

66 ml (100 mmol) of n-butyllithium in hexane were added dropwise, at -78° C., to a solution of 9,7 g (50 mmol) of 1-(2-chlorobenzyl)-1,2,4-triazole and 6 g (50 mmol) of N,N,N',N'-tetramethylethylenediamine in 100 ml of tetrahydrofuran, stirring was carried out for a further half an hour at this temperature and 7.5 g (50 mmol) of adamantanone in tetrahydrofuran were then added so that -70° C. was not exceeded. The reaction mixture was kept at -78° C. for a further 2 hours and then allowed to warm up to room temperature. After working up with water/methylene chloride, 17.4 g of crude product were obtained, and this product gave 10.0 g of pure triazole derivative of melting point 178° C. after recrystallization from ethyl acetate.

Provenance & Evidence