HRID327404

反应详情

EQUATION

反应方程式

HRID 327404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 30 ml of concentrated hydrochloric acid was added 5.00 g of 5-[3-(1-acetylpiperidin-4-yl)-1-oxopropyl]-2,3-dihydrobenzofuran, and the mixture was refluxed for 14 hours. The reaction mixture was left standing for cooling and then made basic with a dilute aqueous solution of sodium hydroxide, followed by extraction with methylene chloride. Organic layers were combined and dried over anhydrous sodium sulfate, then the solvent was distilled off to leave 4.31 g (100%) of 2,3-dihydro-5-[1-oxo-3-(piperidin-4-yl)propyl]benzofuran (4). The solid matter thus obtained was dissolved in methanol, treated with hydrogen chloride and recrystallized from methanol--ethyl acetate to give colorless needles, m.p. 203°-205° C. (decomp.)

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 14 hours
  2. waitThe reaction mixture was left
  3. temperaturefor cooling
  4. extractionfollowed by extraction with methylene chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off