反应详情

温度

160 °C

2-[2-Hydroxy-5-tert-octylphenyl]-2H-benzotriazole (30 g, 0.092 mol), paraformaldehyde (3 g, 0.0955 mol) and di-n-butylamine (24.9 g, 0.191 mol) are charged to a pressure reaction at ambient temperature. The reactor is sealed and the temperature raised to 160° C. The reaction mass is held at 160° C. for four hours and then discharged. The reactor is rinsed with toluene. The toluene, amine and water are stripped by rotary evaporation. The crude product is prepared in a 96% yield (40 g). This product is chromatographed on silica gel using a heptane/ethyl acetate gradient as eluent to remove a trace of unreacted starting benzotriazole intermediate. The title compound is a yellow oil whose structure is confirmed by 1Hnmr.

1. customThe reactor is sealed
2. washThe reactor is rinsed with toluene
3. customThe toluene, amine and water are stripped by rotary evaporation
4. customThis product is chromatographed on silica gel using a heptane/ethyl acetate gradient as eluent
5. customto remove a trace