反应详情

温度

45 °C

3.60 g (=3.67 ml, 20 mmol) of 30% strength NaOCH3 /CH3OH solution were added to a solution of 4.74 g (20 mmol) of 1-amidino-4,4-dimethyl-2-oxoimidazolidine hydrobromide in 47 ml of methanol at room temperature, and the mixture was stirred at 45° C. for 30 min. The solution was then cooled to 20° C. and, at 20° C., 5.97 g (20 mmol) of 2-cyano-3-ethoxyacrylic acid N-methyl-N-(3-trifluoromethylphenyl)amide were added and the mixture was stirred at 20° C. for 20 min, at room temperature for 1.5 hours and while cooling in an icebath for 30 min. The solid which had separated out was filtered off with suction, washed with ether and worked up further as described in Example 1. Likewise, the residue from the filtrate (mother liquor) was further worked up as described in Example 1 and dried. 6.35 g (=77.7% yield) of, according to TLC (CH2Cl2 /C2H5 OH=10:1), virtually pure compound IV were obtained.

1. temperatureThe solution was then cooled to 20° C. and, at 20° C.
2. stirringthe mixture was stirred at 20° C. for 20 min, at room temperature for 1.5 hours
3. temperaturewhile cooling in an icebath for 30 min
4. customThe solid which had separated out
5. filtrationwas filtered off with suction
6. washwashed with ether
7. customdried