HRID1272263

反应详情

EQUATION

反应方程式

HRID 1272263 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of methyl 3,7-dihydroxy-2-naphthoate (2.2 g; 10 mmole), benzylchloride (Merck) (1.26 mL; 11.0 mmole), potassium iodide (1.8 g; 11.0 mmole) and potassium carbonate (2.0 g; 15 mmole) in acetone (30 mL) was refluxed for 7 hours and then cooled to room temperature. The inorganic precipitate was filtered off and washed with acetone, whereas the filtrate was evaporated to dryness The solid residue was dissolved in ethyl acetate and the resulting solution was washed with 1M hydrochloric acid. After drying with sodium sulfate the organic layer was evaporated and the dry residue was recrystallized from methanol, whereat 1.2 g (39%) of methyl-7-benzyloxy-3-hydroxy-2-naphthoate were obtained.

WORKUP

后处理

  1. temperaturewas refluxed for 7 hours
  2. filtrationThe inorganic precipitate was filtered off
  3. washwashed with acetone, whereas the filtrate
  4. customwas evaporated to dryness The solid residue
  5. dissolutionwas dissolved in ethyl acetate
  6. washthe resulting solution was washed with 1M hydrochloric acid
  7. dry with materialAfter drying with sodium sulfate the organic layer
  8. customwas evaporated
  9. customthe dry residue was recrystallized from methanol