HRID639699

反应详情

EQUATION

反应方程式

HRID 639699 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Methyl-3-oxo-pentanoic acid (16.4 g, 126 mmol) was taken up in THF (200 mL) at room temperature under a nitrogen atmosphere, and 1,1-carbonyldiimidazole (22.4 g, 138 mmol) was added in one portion. The reuslting yellow solution was stirred at room temperature for 16 h, and then concentrated in vacuo and the residue diluted with DCM (200 mL). The solution was washed with 2N HCl (100 mL) and water (100 mL) and the aqueous was re-extracted with DCM (50 mL). The combined organics were dried over sodium sulfate and were then concentrated in vacuo to give the title compound as a yellow oil (11.7 g, 80%).

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. additionthe residue diluted with DCM (200 mL)
  3. washThe solution was washed with 2N HCl (100 mL) and water (100 mL)
  4. extractionthe aqueous was re-extracted with DCM (50 mL)
  5. dry with materialThe combined organics were dried over sodium sulfate
  6. concentrationwere then concentrated in vacuo