反应详情

1.10 ml of the triethylamine are added to 1.28 g of 4-[(3-bromophenyl)amino]-7-(3-hydroxy-propyloxy)-6-nitro-quinazoline in 55 ml of methylene chloride. Then, whilst cooling with an ice bath, a solution of 0.47 ml of methanesulphonic acid chloride in 5 ml of methylene chloride is added dropwise. The reaction mixture is stirred for about one hour at ambient temperature. Since some starting material can still be detected, another 20 drops of triethylamine and 10 drops of methanesulphonic acid chloride are added, whilst cooling with an ice bath. The mixture is stirred for a further 30 minutes at ambient temperature, whereupon a clear, reddish-orange solution is formed. For work-up, this is diluted with methylene chloride and added to 100 ml of water. The organic phase is washed with 3% sodium hydrogen carbonate solution and water, dried over sodium sulphate and concentrated by evaporation. A brownish-yellow resin remains, which is further reacted as the crude product. Yield: 1.4 g (92% of theory) Rf value: 0.70 (silica gel, methylene chloride/methanol=9:1)

1. temperatureThen, whilst cooling with an ice bath
2. temperaturewhilst cooling with an ice bath
3. stirringThe mixture is stirred for a further 30 minutes at ambient temperature
4. customwhereupon a clear, reddish-orange solution is formed
5. washThe organic phase is washed with 3% sodium hydrogen carbonate solution and water
6. dry with materialdried over sodium sulphate
7. concentrationconcentrated by evaporation
8. customwhich is further reacted as the crude product