HRID2103949

反应详情

EQUATION

反应方程式

HRID 2103949 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 mmole of 2-mercaptopyrimidine was dissolved in 20 ml of ethanol in stirring. 10 mole of EtOK was added to the solution, stirred for 5 minutes. At last, about 20 mmole (Not more than 30 mmole) of 3-chloropropylene was added, and stirred overnight. The white precipitate was removed by filtration, the solvent in the filtrate was removed in vacuum. The obtained viscous liquid was separated with a Si gel column (solvents: 1 ethylacetate/3 hexane). 1H NMR (CD3Cl): δ(ppm) 8.39 (2H, d, JH-H=4.74), 6.86 (1H, t, JH-H=4.74), 5.89 (1H, m), 5.20 (1H, d, JH-H=17.00), 5.00 (1H, d, JH-H=9.97), 3.71 (2H, d, JH-H=6.83). Yield: 90%.

WORKUP

后处理

  1. stirringstirred for 5 minutes
  2. stirringstirred overnight
  3. customThe white precipitate was removed by filtration
  4. customthe solvent in the filtrate was removed in vacuum
  5. customThe obtained viscous liquid was separated with a Si gel column (solvents: 1 ethylacetate/3 hexane)