反应详情

The solution of 11.3 g of (3-amino-4-methylphenyl)methanol in 500 ml of chloroform is cooled to 0° C. with stirring and admixed with 13.4 ml of triethylamine. 6.03 ml of acetyl chloride are slowly added dropwise. Subsequently, the mixture is stirred at 0° C. over 2 hours. The reaction mixture is poured onto water (1 l) and extracted with dichloromethane (2×350 ml). The organic phases are washed with brine (350 ml), dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a slightly brownish solid from the residue by means of flash chromatography (SiO2 60F). Rf=0.10 (1:2 dichloromethane-diethyl ether); Rt=2.14.

1. stirringSubsequently, the mixture is stirred at 0° C. over 2 hours
2. additionThe reaction mixture is poured onto water (1 l)
3. extractionextracted with dichloromethane (2×350 ml)
4. washThe organic phases are washed with brine (350 ml)
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated by evaporation