HRID634452
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The title compound was made in a similar way as that of the compound of example 21, from tert-butyl 9-trityl-9H-purin-6-ylcarbamate (167 mg, 0.350 mmol), 3-(1-bromopropyl)-4-phenyl-1H-isochromen-1-one (intermediate C20, 100 mg, 0.291 mmol) and 50% dispersion in mineral oil NaH (21 mg, 0.870 mmol) in DMF at 55° C. The crude was purified via reverse phase chromatography with a column stacking of two Biotage C18 30 g SNAP column (Phase A, water 95%, ACN 5%, formic acid 0.1%); Phase B ACN 95%, water 5%, formic acid 0.1%) and further purified by Preparative HPLC (method 1) to give the title compound (2.8 mg, 2.4%) as a colourless solid.
WORKUP
后处理
- customat 55° C
- customThe crude was purified via reverse phase chromatography with a column stacking of two Biotage C18 30 g SNAP column (Phase A, water 95%, ACN 5%, formic acid 0.1%)
- customPhase B ACN 95%, water 5%, formic acid 0.1%) and further purified by Preparative HPLC (method 1)