反应详情

温度

40 °C

A mixture of tert-butyl 4-(5-(2-(4-fluorophenyl)-1,3-dihydroxypropan-2-yl)pyrimidin-2-yl)piperazine-1-carboxylate (650 mg, 1.5 mmol), triphenylphosphine (470 mg, 1.8 mmol), diisopropyl azodicarboxylate (360 mg, 1.8 mmol) and ziram (500 mg, 1.8 mmol) in THF (50 mL) was heated at 40° C. overnight under N2 and concentrated. The residue was diluted with EtOAc (40 mL), washed with water (50 mL*2) and brine, dried over Na2SO4 and concentrated. The residue was purified by Prep-HPLC to give the desired product (35 mg, yield 6%) as a white solid. MS (ES+) C22H27FN4O3 requires: 414. found 359 [M+H−56]+; purity: 93% (UV214).

1. concentrationconcentrated
2. additionThe residue was diluted with EtOAc (40 mL)
3. washwashed with water (50 mL*2) and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by Prep-HPLC