反应详情

温度

25 °C

A solution of 1-trityl-1H-[1,2,4]triazole-3-carboxylic acid {4-[3-butyl-1-(2-fluoro-benzyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide (15 mg, 0.02 mmol) in dichloromethane (1.0 mL) at 25° C. was treated with trifluoroacetic acid (1.0 mL). The resulting solution was stirred at 25° C. for 45 min. At this time, the reaction was treated with triethylsilane (0.003 mL, 0.02 mmol). This solution was stirred at 25° C. for 5 min and then was concentrated in vacuo. The resulting residue was purified by HPLC (20–90% acetonitrile/water (0.075% trifluoroacetic acid in both solvents) over 30 min). Fractions with the desired product were freeze dried to afford 1H-[1,2,4]triazole-3-carboxylic acid {4-[3-butyl-1-(2-fluoro-benzyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide; compound with trifluoro-acetic acid (4.5 mg, 40%) as a white, fluffy solid: EI-HRMS m/e calcd for C26H25N8O3F (M+) 516.2033, found 516.2027.

1. stirringThis solution was stirred at 25° C. for 5 min
2. concentrationwas concentrated in vacuo
3. customThe resulting residue was purified by HPLC (20–90% acetonitrile/water (0.075% trifluoroacetic acid in both solvents) over 30 min)
4. customdried