反应 #582501

ord-a876761294254d60891a607502043b2f

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The mixture was washed with dilute aqueous sodium hydroxide solution (2×300 ml), water (200 ml), brine (300 ml)
  2. 2
    干燥finally with water (250 ml), dried over sodium sulphate
  3. 3
    其他evaporated to dryness

实验过程

4-Hydroxybenzaldehyde (43.4 g, 0.355 mol), dihydropyran (44.4 ml, 0.495 mol), pyridinium p-toluenesulphonate (11.6 g, 0.046 mol, 0.1 mol equiv.) and dichloromethane (300 ml) were stirred for 16 h at room temperature. The mixture was washed with dilute aqueous sodium hydroxide solution (2×300 ml), water (200 ml), brine (300 ml), and finally with water (250 ml), dried over sodium sulphate and evaporated to dryness to leave a dark brown oil(63 g, 87%). This was used without further purification in the following step 1CW02. 1H NMR showed expected signals.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06939479B2uspto-grants-2005_09