HRID1868206

反应详情

EQUATION

反应方程式

HRID 1868206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

That is, 1.5 g of Pd-activated carbon (10%) was weighed in a nitrogen atmosphere and 20 ml of dichloromethane and 1.31 g (4.4 mmol) of 6-(4-benzyloxyphenyl)-2,4-hexanedione were added thereto. The atmosphere in the reaction system was exchanged with hydrogen at 1 atm and stirred at room temperature for 11 hours. The obtained reaction mixture was filtered to remove insoluble matter and the solvent was distilled off under reduced pressure. The residue was charged in a silica gel column and developed first with dichloromethane to remove byproducts. Subsequently, a solution containing a compound eluted from the column with a mixed solvent of 1:1 (by volume ratio) acetone/hexane was concentrated to dryness under reduced pressure to obtain 0.70 g (3.4 mmol) of the objective 6-(4-hydroxyphenyl)-2,4-hexanedione as pale yellow solid. Yield: 77%. Identification was performed by elementary analysis of C and H, and 1H-NMR.

WORKUP

后处理

  1. additionwere added
  2. customThe obtained reaction mixture
  3. filtrationwas filtered
  4. customto remove insoluble matter
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionThe residue was charged in a silica gel column
  7. customto remove byproducts
  8. additionSubsequently, a solution containing a compound
  9. washeluted from the column with a mixed solvent of 1:1 (by volume ratio) acetone/hexane
  10. concentrationwas concentrated to dryness under reduced pressure