HRID339934

反应详情

EQUATION

反应方程式

HRID 339934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 6-amino-2-butoxy-9-{3-[(3-hydroxypropyl)amino]propyl}-7,9-dihydro-8H-purin-8-one (described in WO2007/031726 Example 1 step (viii)) (0.5 g) in NMP, the product from step (i) (0.35 g) was added and the mixture stirred for 10 mins. Sodium triacetoxyborohydride (1.25 g) was then added and stirred at rt for 16 hrs. The reaction mixture was diluted with water and passed through a SCX column, eluted with MeCN/2% NH3 (aq), and solvent removed to give the crude product. The product was purified via RPHPLC to afford the subtitle compound as a solid; 1H NMR DMSO 67.14-7.20 (m, 4H), 6.40 (s, 2H), 4.12 (t, 2H), 3.67 (t, 2H), 3.51 (s, 2H), 3.47 (s, 2H), 3.39 (t, 2H), 2.36-2.44 (m, 4H), 1.78-1.86 (m, 2H), 1.52-1.65 (m, 4H), 1.32-1.41 (m, 2H), 0.90 (t, 3H) MS multimode (+) 487

WORKUP

后处理

  1. stirringstirred at rt for 16 hrs
  2. washeluted with MeCN/2% NH3 (aq), and solvent
  3. customremoved
  4. customto give the crude product
  5. customThe product was purified via RPHPLC