HRID919767

反应详情

EQUATION

反应方程式

HRID 919767 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-dimethylamino-3-ethoxycarbonyl-2-methoxycarbonyl-penta-2,4-dienoic acid methyl ester (14.7 g, 51.7 mmol) and 2,4-dimethoxybenzylamine (8.2 mL, 54.3 mmol) in EtOH (90 mL) was refluxed for 5 h. The mixture was cooled to r.t., concentrated in vacuo, and the residual oil was partitioned between ether and 1 M HCl. The aqueous layer was extracted with additional ether, and the organic layers were combined, washed with water, and dried over MgSO4. Evaporation of the solvent in vacuo afforded 18.4 g of the title compound as a viscous orange oil. MS: (+) m/z 398.23 (M+Na).

WORKUP

后处理

  1. temperaturewas refluxed for 5 h
  2. concentrationconcentrated in vacuo
  3. customthe residual oil was partitioned between ether and 1 M HCl
  4. extractionThe aqueous layer was extracted with additional ether
  5. washwashed with water
  6. dry with materialdried over MgSO4
  7. customEvaporation of the solvent in vacuo