HRID2268928

反应详情

EQUATION

反应方程式

HRID 2268928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 7-methoxy-4-pyridin-4-ylmethyl-2H-phthalazin-1-one (11.4 g, 42.65 mmoles), prepared as described in example 130, and POCl3 (7.95 ml, 85.30 mmoles) in acetonitrile (110 ml) was refluxed for 1.5 hours. Further POCl3 (40 ml) was added and the reflux was kept on overnight. The mixture was dried, dissolved in water, neutralised with NaHCO3, extracted with CH2Cl2 and dried. The residue was chromatographed (eluent: CH2Cl2/CH3OH 97:3) to give 2.9 g of the title compound (yield: 23.8%).

WORKUP

后处理

  1. customprepared
  2. temperaturewas refluxed for 1.5 hours
  3. customThe mixture was dried
  4. dissolutiondissolved in water
  5. extractionextracted with CH2Cl2
  6. customdried
  7. customThe residue was chromatographed (eluent: CH2Cl2/CH3OH 97:3)