HRID582904

反应详情

EQUATION

反应方程式

HRID 582904 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a round bottom flask equipped with an addition funnel and cold water condenser was added, 21.3 grams (0.15 mol.) of diallyl carbonate and 50 mL of tetrahydrofuran and the mixture was stirred. Next, sodium hydride, 8.4 grams (0.21 mol.), was added portion-wise. To the reaction mixture was added, 12.6 grams (0.15 mol.) of cyclopropyl methyl ketone (dissolved in 25 mL of tetrahydrofuran) via the addition funnel. The mixture was heated to relux and heated for an additional 1 hour. Subsequently, the mixture was allowed to cool and the solvent was stripped. Next, cold water (50 mL) and 1 N hydrochloric acid (50 mL) were added. The reaction mixture was transferred to a separatory funnel and diethyl ether was added. The organic layer was dried over MgSO4 and stripped under vacuum to yield the β-ketoester, carboallyloxymethyl cyclopropyl ketone. ##STR13## (B) Preparation of aryl β-triketone

WORKUP

后处理

  1. customTo a round bottom flask equipped with an addition funnel and cold water condenser
  2. additionwas added
  3. additionTo the reaction mixture was added
  4. temperatureThe mixture was heated
  5. temperatureheated for an additional 1 hour
  6. temperatureto cool
  7. customThe reaction mixture was transferred to a separatory funnel
  8. dry with materialThe organic layer was dried over MgSO4