HRID431690

反应详情

EQUATION

反应方程式

HRID 431690 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

To a solution of vinyl acetate (4.3 g, 50 mmol) in dioxane (63 mL) was added 2-(1-hydroxy-ethyl)-3H-pyrimidin-4-one (prepared according to the method of Preparation Twelve, 2.1 g, 15.1 mmol), and the mixture was heated to 50° C. To the resulting solution was added lipase P30 (0.21 9,10 wt %) and the heating was continued for 24 h. The reaction mixture was filtered and the filtrate was evaporated to obtain a thick syrupy liquid residue. The residue was purified by flash column chromatography (95:5 dichloromethane:methanol) to give the title compound as a colorless liquid, 0.97 g (92% of theory). 1H NMR (CDCl3, 300 MHz) δ 1.61 (d, 3H), 2.20 (s, 3H), 5.65 (q, 1H), 6.35 (d, 1H), 7.97 (d, 1H), 11.94 (s, 1H); [α]D+39.9 (c, 1.0, MeOH).

WORKUP

后处理

  1. customprepared
  2. customaccording to the method of Preparation Twelve, 2.1 g, 15.1 mmol), and the mixture
  3. additionTo the resulting solution was added lipase
  4. filtrationThe reaction mixture was filtered
  5. customthe filtrate was evaporated
  6. customto obtain a thick syrupy liquid residue
  7. customThe residue was purified by flash column chromatography (95:5 dichloromethane:methanol)