反应详情

温度

50 °C

To a solution of methyl 3-(6-(4-chlorophenyl)-1,5-dimethyl-2,4-dioxo-1,2-dihydrothieno[2,3-d]pyrimidin-3(4H)-yl)propanoate (See Compound 24, Step 3, 25 mg, 0.064 mmol) in EtOH (1 mL) was added NaBH4 (7.2 mg, 0.19 mmol). The reaction was stirred at 50° C. for 18 h, cooled to RT, quenched with diluted HCl (0.1N, 2 mL) then concentrated to a residue which was purified by Prep HPLC to give 6-(4-chlorophenyl)-3-(3-hydroxypropyl)-1,5-dimethylthieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (10 mg, 43.0% yield) as a white solid. 1H NMR (CD3OD) δ: 7.46-7.45 (m, 4H), 4.10 (t, J=6.8 Hz, 2H), 3.62 (t, J=6.0 Hz, 2H), 3.55 (s, 3H), 2.49 (s, 3H), 1.89-1.86 (m, 2H). LCMS: MH+ 365 and TR=2.742 min.

1. temperaturecooled to RT
2. customquenched with diluted HCl (0.1N, 2 mL)
3. concentrationthen concentrated to a residue which
4. customwas purified by Prep HPLC