HRID443983

反应详情

EQUATION

反应方程式

HRID 443983 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phenylacetonitrile is added to a stirred solution of sodium ethoxide in absolute ethanol (prepared from 1.1 g sodium and 100 ml of ethanol). Next, a solution of 3-formyl-2,2-dimethyl-cyclopropanecarboxylic acid ethyl ester (8.5 g) in absolute ethanol (15 ml) is added over 5 minutes. The reaction mixture is stirred for 12 hours at room temperature and then heated on a steam bath for 0.5 hour. The alcohol is removed in vacuo, and the residue washed with water (250 ml) and ether (150 ml). The aqueous layer is acidified with concentrated hydrochloric acid. The resulting cream colored slurry is filtered and the isolated product dried. The product is dissolved in ether and precipitated with hexane to afford 6.1 g of white crystals, m.p. 186°-188° C.

WORKUP

后处理

  1. temperatureheated on a steam bath for 0.5 hour
  2. customThe alcohol is removed in vacuo
  3. washthe residue washed with water (250 ml) and ether (150 ml)
  4. filtrationis filtered
  5. customthe isolated product dried
  6. dissolutionThe product is dissolved in ether
  7. customprecipitated with hexane