反应详情

温度

120 °C

{3-[2-(tert-Butyl-dimethyl-silanyloxy)-ethoxy]-benzyl}-methyl-amine from Step 3 (294 mg, 1.00 mmol) and 2-chloro-5,6,7-trimethoxy-1H-quinazolin-4-one (prepared as described previously) (270 mg, 1.00 mmol) were dissolved in dry DMSO. Et3N (0.14 mL, 1.00 mmol) was added and the mixture was heated to 120° C. overnight. Upon cooling, the mixture was poured into water and extracted with diethyl ether. The ethereal extracts were dried over Na2SO4 and concentrated in vacuo. The residue was purified by SiO2 eluted with 99:1 CH2Cl2/MeOH to give 435 mg (82.12%) of a white crystalline solid.

1. temperatureUpon cooling
2. extractionextracted with diethyl ether
3. dry with materialThe ethereal extracts were dried over Na2SO4
4. concentrationconcentrated in vacuo
5. customThe residue was purified by SiO2
6. washeluted with 99:1 CH2Cl2/MeOH