HRID2307164

反应详情

EQUATION

反应方程式

HRID 2307164 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(±)-3-[2,4-Bis(methoxymethoxy)phenyl]cyclopentanone (8 mg) was heated at 50° C. in MeOH (3 ml) containing acidic ion exchange resin (0.1 g) for 3 hr. The reaction mixture was filtered and the resin washed with ethyl acetate (20 ml). The filtrate was concentrated in vacuo and the residue purified by flash column chromatography (SiO2, ethyl acetate) to furnish the title compound as a white solid (3.8 mg, 70%). δH (d4-MeOH) 2.52-2.13 (1H, m), 2.26-2.48 (4H, overlapping m), 2.53-2.60 (1H, m), 3.55-3.61 (1H, m), 6.29 (1H, dd), 6.33 (1H, d), 6.96 (1H, d); m/z (ES−) 251 ((M+60)−1)−.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washthe resin washed with ethyl acetate (20 ml)
  3. concentrationThe filtrate was concentrated in vacuo
  4. customthe residue purified by flash column chromatography (SiO2, ethyl acetate)