HRID2171033

反应详情

EQUATION

反应方程式

HRID 2171033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirring solution of 4-(2-Hydroxy-3,4-dimethoxy-phenyl)-indan-1-one (Compound 303) (500 mg, 1.76 mmol) in acetonitrile, were added potassium carbonate (728 mg, 5.28 mmol) and (3-Bromomethyl-oxetan-3-yl)-methanol (764 mg, 4.28 mmol) and the resultant reaction mixture was heated to 70° C. for 16 h. The reaction mixture was quenched with water and extracted with ethyl acetate (3×). The combined ethyl acetate layer was washed with brine and dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification by column chromatography (silica gel, 0-70% ethyl acetate in pet ether) afforded 4-(2-((3-(hydroxymethyl)oxetan-3-yl)methoxy)-3,4-dimethoxyphenyl)-indan-1-one (Compound 104) as a white solid.

WORKUP

后处理

  1. customthe resultant reaction mixture
  2. customThe reaction mixture was quenched with water
  3. extractionextracted with ethyl acetate (3×)
  4. washThe combined ethyl acetate layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulphate
  6. concentrationconcentrated under reduced pressure
  7. customPurification by column chromatography (silica gel, 0-70% ethyl acetate in pet ether)