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 of potassium tert. butoxide are added batchwise, while the temperature should remain below 15° C. The reaction mixture is then stirred for another 30 minutes at 10° C., after which time 31.19 g of 4-[(3-chloro-4-fluoro-phenyl)amino]-7-fluoro-6-nitro-quinazoline are added batchwise, while again the temperature should not exceed 15° C. The deep red reaction mixture is stirred for another hour at 15° C. For working up, the mixture is poured onto 2.5 l of water and neutralised with 2N hydrochloric acid. The yellowish precipitate formed is suction filtered, washed with water and dried at 50° C. in a drying cupboard.

1. customshould remain below 15° C
2. customexceed 15° C
3. customThe deep 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