HRID1022416

反应详情

EQUATION

反应方程式

HRID 1022416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

3-Hydroxy-isophthalic acid di-tert-butyl ester (90 mg, 0.3 mmol) was dissolved in dry acetone (5 ml), K2CO3 (90 mg, 0.65 mmol) and methyl 10-bromodecanoate (0.075 ml, 0.3 mmol) was added. The mixture was heated to reflux. The heating caused dissolution of the K2CO3. After a while, a precipitate was formed. Reflux (50° C.) was continued over night. More K2CO3 (30 mg, 0.2 mmol) and methyl 10-bromodecanoate (0.025 ml, 0.1 mmol) was added. The mixture was refluxed at 50° C. over night. To the dry reaction mixture EtOAc and water was added. After extraction, the organic layer was washed with water and brine, dried (Na2SO4) and concentrated to give the crude title compound as a clear oil.

WORKUP

后处理

  1. temperatureThe mixture was heated to reflux
  2. customAfter a while, a precipitate was formed
  3. waitwas continued over night
  4. temperatureThe mixture was refluxed at 50° C. over night
  5. additionwas added
  6. extractionAfter extraction
  7. washthe organic layer was washed with water and brine
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated