HRID2297482

反应详情

EQUATION

反应方程式

HRID 2297482 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-(6-methoxy-4-oxo-3,4-dihydro-phthalazin-1-yl)-butyric acid methyl ester (9.23 g, 0.034 moles), prepared as described in example 113, and POCl3 (1.87 ml, 0.2 mole) in acetonitrile (100 ml) was refluxed. After 1.5 hours the mixture was dried, taken up in water and neutralised with NaHCO3. The mixture was extracted with ethyl acetate and the organic phase dried to give a residue which was chromatographed (eluent: petrolatum/ethyl acetate 7:3). There were yielded 7.4 g of the title compound (yield: 63.9%).

WORKUP

后处理

  1. customprepared
  2. temperaturewas refluxed
  3. customAfter 1.5 hours the mixture was dried
  4. extractionThe mixture was extracted with ethyl acetate
  5. customthe organic phase dried
  6. customto give a residue which
  7. customwas chromatographed (eluent: petrolatum/ethyl acetate 7:3)