HRID66142

反应详情

EQUATION

反应方程式

HRID 66142 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4,7-Dihydro-4,7-dioxo-6-hydroxy-1H-cyclohepta[b]pyridine-2-carboxylic acid ethyl ester (12.0 g, described in Example 3) is added to a stirring mixture of sodium hydride (57%, 2.8 g) and dimethylformamide (400 ml) at room temperature. Ethyl bromoacetate (15.8 g) is added. The mixture is stirred at room temperature for 20 hr and poured on ice. Water is added and the mixture is extracted with chloroform. The organic extract is dried over sodium sulfate and evaporated. The residue is crystallized from ethyl acetate to give the title compound, mp 186°-188° C.

WORKUP

后处理

  1. additionpoured on ice
  2. extractionthe mixture is extracted with chloroform
  3. extractionThe organic extract
  4. dry with materialis dried over sodium sulfate
  5. customevaporated
  6. customThe residue is crystallized from ethyl acetate