HRID2171030

反应详情

EQUATION

反应方程式

HRID 2171030 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a stirring solution of 4-[2-(3-Hydroxymethyl-oxetan-3-ylmethoxy)-3,4-dimethoxy-phenyl]-indan-1-one (Compound 104)(100 mg, 0.2604 mmol) in dichloromethane (15 mL), were added triethylamine (0.1 mL, 0.772 mmol) and ethyl isocyanate (55 mg, 0.78 mmol) and the resultant reaction mixture was heated to 50° C. for 16 h. The reaction mixture was quenched with sodium bi carbonate solution and extracted with dichloromethane (3×). The combined dichloromethane layer was washed with brine and dried over anhydrous sodium sulphate and concentrated under reduced pressure. Purification by column chromatography (silica gel, 0-25% ethyl acetate in pet ether) to afforded the title compound as a solid.

WORKUP

后处理

  1. customthe resultant reaction mixture
  2. customThe reaction mixture was quenched with sodium bi carbonate solution
  3. extractionextracted with dichloromethane (3×)
  4. washThe combined dichloromethane 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, 0-25% ethyl acetate in pet ether)