HRID872542

反应详情

EQUATION

反应方程式

HRID 872542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 5-(2-hydroxypropan-2-yl)isoxazole-3-carboxylate (0.436 g, 2.189 mmol) was dissolved in methanol (20 ml). A solution of cesium carbonate (1.426 g, 4.38 mmol) in 20 ml of water was added and the reaction mixture was stirred at RT for 18 h. Solvents were evaporated and the residue was taken into a mixture of ethyl acetate and water, pH was adjusted to 2.5 with 10% citric acid solution and the layers were separated. Water layer was extracted three times with ethyl acetate and the combined organic layers were dried with Na2SO4, filtered and evaporated affording 0.246 g of the title compound. 1H-NMR (400 MHz; d6-DMSO): δ 1.49 (s, 6H), 5.75 (m, 1H), 6.60 (s, 1H).

WORKUP

后处理

  1. customSolvents were evaporated
  2. additionthe residue was taken into a mixture of ethyl acetate and water, pH
  3. customthe layers were separated
  4. extractionWater layer was extracted three times with ethyl acetate
  5. dry with materialthe combined organic layers were dried with Na2SO4
  6. filtrationfiltered
  7. customevaporated