反应详情

4-{5-[2-(2,2,6,6-Tetramethyl-piperidin-4-ylamino)-pyrimidin-4-yl]-thiophen-2-yl}-piperazine-1-carboxylic acid ethyl ester (120 mg, 0.25 mmol) in chloroform (5 ml) was treated with Me3SiI (0.34 ml, 2.5 mmol) at 60° C. for 4 hours. 6N-HCl in propanol (5 ml) was added and stirred for 30 minutes at room temperature. The reaction mixture was poured on 2N-NaOH and extracted 5 times with EtOAc. The combined organic phases were dried over sodium sulfate, filtered, and purified via chromatography on silicagel (TBME/MeOH/ammonia:95/4.5/0/5 to 80/18/2) to give the title compound as yellow crystals. Yield: 20 mg (20%).

1. extractionextracted 5 times with EtOAc
2. dry with materialThe combined organic phases were dried over sodium sulfate
3. filtrationfiltered
4. custompurified via chromatography on silicagel (TBME/MeOH/ammonia:95/4.5/0/5 to 80/18/2)