HRID1616921

反应详情

EQUATION

反应方程式

HRID 1616921 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 7-methoxy-4a-methyl-3,4,4a,9a-tetrahydro-2Hbenzo[4,5]furo[2,3-c]pyridine-1-one (1.0 g, 4.30 mmol) in tetrahydrofuran (3 mL) was slowly added 1.0 M of lithium tetrahydroaluminate in tetrahydrofuran (2 mL). After 30 min stirring another portion of 1.0 M of lithium tetrahydroaluminate in tetrahydrofuran (1 mL) was added and the reaction was stirred for 2 h. The reaction was transferred into ice, 6N aqueous HCl was added followed by ethyl acetate. The aqueous layer was basified by adding NaOH and the product was extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, filtered and the solvent was evaporated to provide a colorless oil. The product was used in the next reaction step without further purification.

WORKUP

后处理

  1. additionwas added
  2. additionwas added
  3. extractionthe product was extracted with ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent was evaporated
  8. customto provide a colorless oil
  9. customThe product was used in the next reaction step without further purification