反应详情

To a solution of 2,4,5-trichloropyrimidine (484.9 mg, 2.64 mmol) and 6-(methylamino)hexahydrofuro[3,2-b]furan-3-ol (530.2 mg, 3.33 mmol) in EtOH (30 mL) was added Et3N (566.0 mg, 5.59 mmol). After addition, the reaction mixture was stirred at rt overnight and concentrated in vacuo. The residue was dissolved in a mixture of EtOAc and water (1/1 (v/v), 100 mL) and extracted with EtOAc (100 mL×3). The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2SO4, concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/PE (v/v)=1/2) to give the title compound as a pale yellow solid (760.2 mg, 94.0%).

1. additionAfter addition
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was dissolved in a mixture of EtOAc and water (1/1 (v/v), 100 mL)
4. extractionextracted with EtOAc (100 mL×3)
5. washThe combined organic phases were washed with brine (100 mL)
6. dry with materialdried over anhydrous Na2SO4
7. concentrationconcentrated in vacuo
8. customThe residue was purified by silica gel column chromatography (EtOAc/PE (v/v)=1/2)