HRID872895

反应详情

EQUATION

反应方程式

HRID 872895 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 5-(2-oxopropyl)isoxazole-3-carboxylate (0.65 g, 3.30 mmol) was dissolved in ethanol (10 ml). A solution of cesium carbonate (1.611 g, 4.94 mmol) in water (5 ml) was added to the reaction mixture and it was stirred for 7 h at RT. The reaction mixture was concentrated, diluted with water and pH was adjusted to 2 with citric acid. The aqueous phase was extracted with ethyl acetate, dried with Na2SO4 and evaporated to dryness afforded 0.203 g (36%) of the title compound. 1H-NMR (400 MHz; d6-DMSO): δ, 2.21 (s, 3H), 4.20 (s, 2H), 6.67 (s, 1H).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with water and pH
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialdried with Na2SO4
  5. customevaporated to dryness