反应详情

A mixture of 2-hydroxymethyl-1-undecanol (10 mmole) HFPP (10 mmole) and p-toluenesulphonic acid (50 mg) in toluene (50 ml) was heated at reflux while allowing water to distil out. When reaction was complete the excess toluene was removed by distillation and the product allowed to cool before dilution with dichloromethane. After washing with saturated NaHCO3 solution the mixture was distilled to give a colourless liquid identified as NDPP by IR, 1H NMR and mass spectroscopy and elemental analysis (yield: 68%; bp: 230°-40° C. at 0.3 mbar; SOR: 5.9,c=3). The product was a 85:15 mixture of the trans and cis isomers.

1. temperaturewas heated
2. temperatureat reflux
3. customto distil out
4. customWhen reaction
5. customwas removed by distillation
6. temperatureto cool before dilution with dichloromethane
7. washAfter washing with saturated NaHCO3 solution the mixture
8. distillationwas distilled
9. customto give a colourless liquid
10. additiona 85:15 mixture of the trans and cis isomers