HRID623997

反应详情

EQUATION

反应方程式

HRID 623997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of methyl 5-(pyrimidin-4-yl)oxazole-4-carboxylate (179 mg, 0.80 mmol) in THF/H2O (1:1, 6 mL) was treated with LiOH (60 mg, 1.43 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 15 min, then diluted with EtOAc and 1N aq. HCl-solution was added (to reach pH=1). The layers were separated and the aq. layer extracted with EtOAc (2×), EtOAc/MeOH 4:1 then DCM/MeOH 4:1. The combined organic extracts were dried (Na2SO4), filtered and concentrated in vacuo to obtain the title compound as a solid which was used without further purification. LC-MS conditions A: tR=0.56 min, [M+H]+=192.47.

WORKUP

后处理

  1. additionwas added (to reach pH=1)
  2. customThe layers were separated
  3. extractionthe aq. layer extracted with EtOAc (2×), EtOAc/MeOH 4:1
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo