反应详情

温度

120 °C

A mixture of 1-[3-phenyl-1-(toluene-4-sulfonyl)-1H-indol-2-yl]ethylamine (294 mg, 0.753 mmol), 6-chloro-9H-purine (140 mg, 0.903 mmol) and DIPEA (0.20 mL, 1.13 mmol) in n-butanol (1.5 mL) was stirred in a sealed tube for 56 h at 120° C. After cooling to RT, the crude reaction mixture was loaded onto an Isolute® SCX-2 cartridge which was washed with MeOH and the product eluted with 2M NH3/MeOH. The product containing fractions were combined and concentrated under reduced pressure. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-7% 2M NH3/MeOH in DCM) affording N-(1-(3-phenyl-1-tosyl-1H-indol-2-yl)ethyl)-9H-purin-6-amine as a yellow solid (350 mg, 91%). LCMS: RT 3.31 min [M+H]+ 509.1

1. temperatureAfter cooling to RT
2. customthe crude reaction mixture
3. washwas washed with MeOH
4. washthe product eluted with 2M NH3/MeOH
5. additionThe product containing fractions
6. concentrationconcentrated under reduced pressure
7. customThe resulting residue was purified by column chromatography (Si—PCC, gradient 0-7% 2M NH3/MeOH in DCM)