反应详情

温度

80 °C

2-(2H-Benzotriazol-2-yl)-6-chloromethyl-4-methyl-phenol (10.0 g, 33 mmol) is suspended in a mixture of isoamyl alcohol (35 g, 0.4 mol) and acetone (5 g) and stirred at 80° C. for 30 minutes. Sodium carbonate (4.7 g, 44 mmol) is added and the slightly yellow reaction mixture is stirred at 80° C. for 30 minutes. Acetone is removed under vacuum, salts are filtered off and the reaction mixture is evaporated to dryness. The residue is dissolved in ethyl acetate and extracted with aqueous citric acid (5%) and brine. The organic layer is dried over sodium sulphate, filtered and evaporated to dryness. The crude product is purified by column chromatography (ethyl acetate/heptane 1:12) to yield 7.0 g of 2-(2H-Benzotriazol-2-yl)-6-(3-methyl-butoxymethyl)-4-methyl-phenol.

1. stirringthe slightly yellow reaction mixture is stirred at 80° C. for 30 minutes
2. customAcetone is removed under vacuum, salts
3. filtrationare filtered off
4. customthe reaction mixture is evaporated to dryness
5. dissolutionThe residue is dissolved in ethyl acetate
6. extractionextracted with aqueous citric acid (5%) and brine
7. dry with materialThe organic layer is dried over sodium sulphate
8. filtrationfiltered
9. customevaporated to dryness
10. customThe crude product is purified by column chromatography (ethyl acetate/heptane 1:12)