反应详情

At 10° C., 56.4 ml (0.789 mol) of acetylchloride are added dropwise to a suspension of 210.6 g (0.608 mol) of (2) and 176 ml of N-ethyldiisopropylamine (0.95 mol) in 2.1 l of ethyl acetate. The mixture is stirred for 90 minutes at ambient temperature and then washed 3 times with 700 ml of water at 60° C. The organic phase is evaporated down and combined with 590 ml of ethanol. The mixture is briefly brought to boiling point, cooled to 0-5° C. and stirred at this temperature for 30 minutes. The product that crystallises out is filtered off and dried at 60° C. in vacuo. Yield: 180.3 g (76.3%), melting point: 177.6° C.

1. washwashed 3 times with 700 ml of water at 60° C
2. customThe organic phase is evaporated down
3. temperaturecooled to 0-5° C.
4. stirringstirred at this temperature for 30 minutes
5. customThe product that crystallises out
6. filtrationis filtered off
7. customdried at 60° C. in vacuo