反应详情

A solution of {4-[5-(3-Amino-3-methyl-but-1-ynyl)-thiophen-2-yl]-pyrimidin-2-yl}-(2,2,6,6-tetramethyl-piperidin-4-yl)-amine (Example 5, 100 mg, 0.252 mmol) in 10 ml of THF and LAH (1M in THF, 0.25 ml, 0.25 mmol) was refluxed for 3 hours, poured on water and extracted 3 times with TBME. The combined organic phases were dried over sodium sulfate, filtered and purified via chromatography on silicagel (DCM/MeOH/ammonia:90/10/1 to 85/15/2) to give the title compound as yellow solid. Yield: 20 mg (20%).

1. additionpoured on water
2. extractionextracted 3 times with TBME
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. filtrationfiltered
5. custompurified via chromatography on silicagel (DCM/MeOH/ammonia:90/10/1 to 85/15/2)