HRID59115

反应详情

EQUATION

反应方程式

HRID 59115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methanol (1.06 g, 33.1 mmol) and sodium hydroxide (5 M (aq), 2.0 mL, 9.94 mmol) were added to a solution of (2-chloro-6-(1-ethoxyvinyl)pyrimidin-4-yl)methyl methanesulfonate (1.94 g, 6.63 mmol) in benzene (25 mL). Tetrabutylammonium hydrogen sulfate (0.225 g, 0.66 mmol) was added. The mixture was stirred vigorously at rt for 6 h. The phases were separated and the organic phase was filtered through a short silica plug which was washed with 10% MeOH in EtOAc (75 mL) and the solvent was evaporated. The residue was purified by preparative HPLC to give the title compound 0.287 g (19%).

WORKUP

后处理

  1. customThe phases were separated
  2. filtrationthe organic phase was filtered through a short silica plug which
  3. washwas washed with 10% MeOH in EtOAc (75 mL)
  4. customthe solvent was evaporated
  5. customThe residue was purified by preparative HPLC