反应详情

温度

130 °C

2.50 g of 2-chloro-6,7-dimethoxy-4-(3-nitrophenyl)quinazoline obtained in Production Example 1,4.89 g methylamine hydrochloride and 11.0 g triethylamine were suspended in 25 ml 1-methyl-2-pyrrolidinone and stirred at 130° C. for 18 hours in a sealed tube. Ethyl acetate and tetrahydrofuran were added thereto, and the reaction solution was washed with water 5 times and then with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (hexane:ethyl acetate=1:2). The product was recrystallized from tetrahydrofuran-ethyl acetate to give 1.89 g of the title compound as yellow crystals.

1. washthe reaction solution was washed with water 5 times
2. dry with materialwith brine and dried over anhydrous magnesium sulfate
3. customThe solvent was evaporated
4. customthe crude product was purified
5. customseparated by silica gel column chromatography (hexane:ethyl acetate=1:2)
6. customThe product was recrystallized from tetrahydrofuran-ethyl acetate