HRID840612
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-methyl-1-(2′,3′5′-tri-O-benzoyl-β-D-ribofuranosyl)-pyrimidin-4-one (13.86 g, 25 mmol) in methanol (150 ml) was added 4.37 N sodium methoxide solution in MeOH (2.5 mmol, 0.1 eq.). The solution was stirred overnight at room temperature and then evaporated. The residue was partitioned between water (100 ml) and dichloromethane (2×150 ml). The aqueous layer was neutralized with Dowex 50H+-form and evaporated. The orange oily residue was crystallized from ethanol/acetone 3:1 to give the title compound (2.37 g, 39%). 1H-NMR (CDCl3): δ8.1 (d, 1H, H6); 6.0 (d, 1H, H5); 5.65 (m, 2H, H1′, 2′-OH); 5.25, 5.2 (d,t, 2H, 3′-OH, 5′-OH); 2.45 (s, 3H, CH3)
WORKUP
后处理
- customevaporated
- customThe residue was partitioned between water (100 ml) and dichloromethane (2×150 ml)
- customevaporated
- customThe orange oily residue was crystallized from ethanol/acetone 3:1