反应详情

温度

10 °C

29.36 g of cyclopropylmethanol are dissolved in 310 ml of N,N-dimethylformamide and cooled to about 10° C. in an ice bath. Then 41.58 g potassium tert-butoxide is added in batches, while the temperature should stay below 15° C. The reaction mixture is then stirred for another 30 minutes at 10° C., then 31.19 g of 4-[(3-chloro-4-fluorophenyl)amino]-7-fluoro-6-nitroquinazoline is added in batches, while again the temperature should not exceed 15° C. The dark red reaction mixture is stirred for another hour at 15° C. For working up, the mixture is poured onto 2.5 1 of water and neutralized with 2N hydrochloric acid. The yellowish precipitate formed is suction filtered, washed with water, and dried at 50° C. in a drying cupboard. Yield: 36.02 g (100% of theory); melting point: 204° C.; mass spectrum (ESI+): m/z=389, 391 [M+H]+.

1. customshould stay below 15° C
2. customexceed 15° C
3. customThe dark red reaction mixture
4. stirringis stirred for another hour at 15° C
5. customThe yellowish precipitate formed
6. filtrationfiltered
7. washwashed with water
8. customdried at 50° C. in a drying cupboard