HRID234975

反应详情

EQUATION

反应方程式

HRID 234975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

5'-O-(t-Butyldimethylsilyl)-2',3'-dideoxy-5-methyl-2'-oxo-uridine (3.854 g, 10.9 mmol) from Step 3 was dissolved in 50 mL of dry dimethylformamide (DMF) and 1.74 mL (1.56 g, 13.1 mmol) of N,N-dimethylformamide dimethylacetal was added. The reaction mixture was heated in an oil bath at 50° C. for 40 min. The solvent was evaporated in vacuo and the residue purified on a silica gel column, the product eluting with 5% methanol in methylene chloride to give 2.512 g (56.3% yield) of the title compound, [α]D23 =-84.2° (c, 1.44, MeOH). DCI MS M/Z: (M+H)+ 410.

WORKUP

后处理

  1. customThe solvent was evaporated in vacuo
  2. customthe residue purified on a silica gel column
  3. washthe product eluting with 5% methanol in methylene chloride