反应详情

A mixture of 2.6 g (0.010 mol) of (1,1'-biphenyl-4-yl)chloromethyldimethylsilane and 1.1 g (0.012 mol) of 1,2,4-triazole sodium salt in 5 ml of dimethylformamide was warmed to 80°-90° for 2 hours, cooled, diluted with water, and extracted with ether. The ether solution was washed with water and brine, dried over magnesium sulfate, and evaporated to leave 2.3 g of colorless solid, m.p. 79°-86°. Recrystallization from a mixture of 25 ml of hexanes and 2 ml of ethyl acetate gave 1.1 g (38%) of the title compound: m.p. 92°-93°; ir (Nujol®) 1255, 1130, 1000, 825, 760, 695 cm-1 ; nmr (CDCl3) 0.4 (6H, s), 3.9 (2H, s), 7.2-7.7 (9H, m), 7.8 (1H, s), 7.9 (1H, s); analysis for C17H19N3Si (mw 293.43):

1. temperaturewas warmed to 80°-90° for 2 hours
2. temperaturecooled
3. extractionextracted with ether
4. washThe ether solution was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. customevaporated