反应详情

温度

45 °C

1-(5-chloro-2-hydroxyphenyl)ethanone, (165 g, 0.967 mol) was slurried in 2-propanol (1000 mL) then 1,1-dimethoxy-N,N-dimethylmethanamine (258.28 mL, 1.93 mol) was added and the resulting yellow solution was stirred at 45° C. for 18 hours. The resulting suspension was cooled to room temperature and stirred for a further 48 hours. The solid was filtered off, washed with 2-propanol (2×200 mL) and then tert-butylmethyl ether (200 mL) then dried to give the title compound as a bright yellow solid, (204.59 g).

1. temperatureThe resulting suspension was cooled to room temperature
2. stirringstirred for a further 48 hours
3. filtrationThe solid was filtered off
4. washwashed with 2-propanol (2×200 mL)
5. dry with materialtert-butylmethyl ether (200 mL) then dried