HRID2240769

反应详情

EQUATION

反应方程式

HRID 2240769 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 3-(4-formyl-2,6-dimethyl-phenyl)-acrylic acid (2.2 g, 10.8 mmol) and DIPEA (2.0 mL, 11.9 mmol) in ethanol (80 mL), Pd/C (200 mg, 10% Pd, moistened with 50% water) is added. The suspension is vigorously stirred under 1 bar of H2 for 1 h. The mixture is filtered over Celite and the filtrate is evaporated. The residue is poured onto 1 N aq. HCl/ice and extracted with EA. The organic extract is washed once with 1 N aq. HCl and once with brine, dried over MgSO4, filtered and evaporated to give 3-(4-hydroxymethyl-2,6-dimethyl-phenyl)-propionic acid (2.2 g) as a pale yellow resin; LC-MS: tR=0.71 min.

WORKUP

后处理

  1. filtrationThe mixture is filtered over Celite
  2. customthe filtrate is evaporated
  3. additionThe residue is poured onto 1 N aq. HCl/ice
  4. extractionextracted with EA
  5. extractionThe organic extract
  6. washis washed once with 1 N aq. HCl and once with brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customevaporated