反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 25 °C
PROCEDURE
实验过程
A solution of 1-trityl-1H-imidazole-4-carboxylic acid {4-[3-butyl-1-(2-fluoro-benzyl)-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-ylmethyl]-phenyl}-amide (46 mg, 0.06 mmol) in dichloromethane (1.0 mL) at 25° C. was treated with trifluoroacetic acid (1.0 mL). The reaction was stirred at 25° C. for 30 min. At this time, the reaction was treated with triethylsilane (20 μL, 0.12 mmol) and then concentrated in vacuo. The resulting residue was purified by HPLC (20–95% acetonitrile/water (0.075% trifluoroacetic acid in both solvents) over 20 min). Fractions with the desired product were freeze dried to afford 1H-imidazole-4-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 (27.8 mg, 74%) as a white solid: EI-HRMS m/e calcd for C27H26N7O3F (M+) 515.2081, found 515.2083.
WORKUP
后处理
- concentrationconcentrated in vacuo
- customThe resulting residue was purified by HPLC (20–95% acetonitrile/water (0.075% trifluoroacetic acid in both solvents) over 20 min)
- customdried