HRID520409

反应详情

EQUATION

反应方程式

HRID 520409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 4-methylenecyclohexanecarboxylate (2 g, 11.89 mmol) in ether (40 mL) was added LAH (0.5 g, 13.17 mmol) portionwise under N2. The reaction mixture was refluxed for 1 h and was quenched by addition of 1 mL of EtOAc carefully and refluxed for 10 min. The reaction mixture was cooled down and added 3 mL of 1 N NaOH and stirred for 5 min, filtered off the solid and washed with ether. The filtration was washed with water, brine, dried (MgSO4), and removed the solvent to afford (4-methylenecyclohexyl)methanol.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 1 h
  2. customwas quenched by addition of 1 mL of EtOAc carefully
  3. temperaturerefluxed for 10 min
  4. temperatureThe reaction mixture was cooled down
  5. additionadded 3 mL of 1 N NaOH
  6. filtrationfiltered off the solid
  7. washwashed with ether
  8. filtrationThe filtration
  9. washwas washed with water, brine
  10. dry with materialdried (MgSO4)
  11. customremoved the solvent