反应详情

8.0 g (20 millimoles) of 1-(4-carbomethoxyphenyl)-4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthalenyl)-butane-1,4-dione (for preparation see Example 9) and 5.5 g (0.1 mole) of ammonium chloride in 150 ml of dry dimethylformamide were heated for 6 hours at 150° C. After cooling, the mixture was poured onto water and the precipitated crystals were filtered off under suction, washed several times with water and dried in a stream of nitrogen. Purification by column chromatography (silica gel; n-heptane plus increasing amounts of ethyl acetate) and recrystallization from ethanol gave 3.6 g of the title compound of melting point 176°-179° C.

1. temperatureAfter cooling
2. additionthe mixture was poured onto water
3. filtrationthe precipitated crystals were filtered off under suction
4. washwashed several times with water
5. customdried in a stream of nitrogen
6. customPurification
7. temperatureby column chromatography (silica gel; n-heptane plus increasing amounts of ethyl acetate) and recrystallization from ethanol