HRID385868

反应详情

EQUATION

反应方程式

HRID 385868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a three neck 3 L round bottom flask was added 1,1-bis(bromomethyl)cyclobutane (100 g, 0.43 mol), potassium carbonate (285 g, 2.06 mol), acetonitrile (1000 mL) and ethanolamine (37.8 g, 0.62 mol). The reaction mixture was heated to reflux for 2 days. The reaction mixture was concentrated to half volume and water was added (300 mL). The aqueous layer was extracted with dichloromethane (2×500 mL). The combined organic layers were washed with brine (200 mL), dried over sodium sulfate, filtered, and concentrated to afford the title compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 2 days
  3. concentrationThe reaction mixture was concentrated to half volume and water
  4. additionwas added (300 mL)
  5. extractionThe aqueous layer was extracted with dichloromethane (2×500 mL)
  6. washThe combined organic layers were washed with brine (200 mL)
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated