HRID67267

反应详情

EQUATION

反应方程式

HRID 67267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

360 g of a 30% solution of sodium methylate in methanol are added dropwise to a suspension of 134 g of terephthalaldehyde in 500 ml of methanol at 20°-25° C. 191 g of 2-(diethylphosphoryl)-propionitrile [prepared by the method of M. L. Raggio and D. S. Watt, J. Org. Chem. 41, 1873 (1976)] are now slowly added dropwise to the resulting reaction solution at 20°-25° C. The reaction mixture is stirred at room temperature for 6 hours and then poured onto 1,000 ml of water, and the aqueous suspension is adjusted to a pH value of 7 with acetic acid. The product which has precipitated is filtered off, dried and then chromatographed on silica gel. 35 g (20.5% of theory) of 2-methyl-3-(4-formylphenyl)-2-propenonitrile of the formula ##STR32## and then obtained in the form of colourless crystals having a melting point of 63°-64° C.

WORKUP

后处理

  1. addition41, 1873 (1976)] are now slowly added dropwise to the resulting reaction solution at 20°-25° C
  2. customThe product which has precipitated
  3. filtrationis filtered off
  4. customdried
  5. customchromatographed on silica gel