反应详情

N-[7-[2-(2-amino-propionylamino)-ethoxy]-4-(4-bromo-2-fluoro-phenylamino)-quinazolin-6-yl]-acrylamide (30 mg, 0.06 mmol) and 37 weight % of formaldehyde (9 μl, 0.12 mmol) were diluted with THF (1 ml) and methanol (1 ml), and stirred at room temperature for 10 min. Sodium cyanoborohydride (11 mg, 0.17 mmol) was added thereto, and the solution was stirred for 4 hours. The resulting solution was distilled under a reduced pressure to remove the solvent, saturated sodium bicarbonate aqueous solution (20 ml) was added thereto, and extracted with chloroform (20 ml) twice. The separated organic layer was dried over magnesium sulfate, filtered and distilled under a reduced pressure, and resulting impure residue was subjected to column chromatography to obtain the title compound 23 mg (yield: 73%).

1. stirringthe solution was stirred for 4 hours
2. distillationThe resulting solution was distilled under a reduced pressure
3. customto remove the solvent, saturated sodium bicarbonate aqueous solution (20 ml)
4. additionwas added
5. extractionextracted with chloroform (20 ml) twice
6. dry with materialThe separated organic layer was dried over magnesium sulfate
7. filtrationfiltered
8. distillationdistilled under a reduced pressure
9. customresulting impure residue