HRID60366

反应详情

EQUATION

反应方程式

HRID 60366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 3-(5-(4-chlorobenzyl)-7-(3-chlorophenyl)-1-methyl-2,4-dioxo-1H-pyrrolo[3,2-d]pyrimidin-3(2H,4H,5H)-yl)propyl acetate (50 mg, 0.1 mmol) in THF (0.5 mL) and water (0.5 mL) was added LiOH.H2O (8.4 mg, 0.2 mmol). The reaction was stirred at RT for 30 min then diluted with EA (5 mL). The organic layer was washed with brine (5 mL), dried over Na2SO4 and concentrated to a residue which was purified by Prep HPLC to give 5-(4-chlorobenzyl)-7-(3-chlorophenyl)-3-(3-hydroxypropyl)-1-methyl-1H-pyrrolo[3,2-d]pyrimidine-2,4(3H,5H)-dione (20 mg, 41% yield). 1H NMR (CDCl3) δ: 7.39-7.29 (m, 5H), 7.25-7.17 (m, 3H), 6.91 (s, 1H), 5.56 (s, 2H), 4.28-4.15 (m, 2H), 3.62 (s, 1H), 3.52 (d, J=4.8 Hz, 2H), 3.21 (s, 3H), 1.96-1.82 (m, 2H). LCMS: MH+ 458 and TR=2.953 min.

WORKUP

后处理

  1. washThe organic layer was washed with brine (5 mL)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated to a residue which
  4. customwas purified by Prep HPLC