反应详情

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0 °C

To a solution of methyl 2-methyl-2-(4-((9-methyl-2-(2-methyl-1H-benzo[d]imidazol-1-yl)-6-morpholino-9H-purin-8-yl)methyl)piperidin-1-yl)propanoate 507 (0.10 g, 0.183 mmol) in THF (10 mL) was added a 1.0 M solution of lithium aluminum hydride in THF (0.18 mL, 0.18 mmol) at 0° C. The reaction was stirred at 0° C. for 1 hour. The reaction was then quenched by adding 2 mL of sat. NH4Cl solution. The cloudy mixture was then loaded onto an ISOLUTE® SCX-2 column. The column was first washed with MeOH prior to eluting the product by adding 2M NH3 in MeOH. The crude product was then concentrated and purified by RP-HPLC to give 509. LCMS m/z: 519.3 (MH+)

1. customThe reaction was then quenched
2. additionby adding 2 mL of sat. NH4Cl solution
3. washThe column was first washed with MeOH
4. washto eluting the product
5. additionby adding 2M NH3 in MeOH
6. concentrationThe crude product was then concentrated
7. custompurified by RP-HPLC