HRID2300041

反应详情

EQUATION

反应方程式

HRID 2300041 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 1,3-dibenzylbarbituric acid 154 mg (0.500 mmol) in dry dichloromethane 2.0 mL under a nitrogen atmosphere, added was pyridine 1.0 mL (12 mmol) and stirred at 0° C. Added was 2-thienylacetyl chloride 80 mg (0.50 mmol, 1.00 equivalent) in dichloromethane 1.0 mL to the solution slowly during a period of 20 minutes, then stirred at room temperature for 3 hours. Added was ether 50 mL and washed the organic layer with 2 M hydrochloric acid and saturated brine, and dried over sodium sulfate. Purified was the crude product 216 mg after removal of the solvent under the reduced pressure, by column chromatography (silica gel, eluted with dichloromethane). It obtained 1,3-dibenzyl-5-(2-thienylacetyl)barbituric acid 153 mg as yellow viscous oil (56.9% yield).

WORKUP

后处理

  1. additionAdded
  2. customof 20 minutes
  3. stirringstirred at room temperature for 3 hours
  4. additionAdded
  5. washwashed the organic layer with 2 M hydrochloric acid and saturated brine
  6. dry with materialdried over sodium sulfate
  7. customPurified
  8. customafter removal of the solvent under the reduced pressure
  9. washby column chromatography (silica gel, eluted with dichloromethane)