HRID2268924

反应详情

EQUATION

反应方程式

HRID 2268924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension under N2 of 4-furan-2-ylmethyl-7-methoxy-2H-phthalazin-1-one (1.8 g, 7.02 mmoles), prepared as described in example 126, in acetonitrile (40 ml) was added under stirring with POCl3 (3.27 ml, 35.1 mmoles), and refluxed for 1 hour, then dried. The residue was suspended in water (50 ml), added with NaHCO3 up to alkalinity, and stirred for 30 minutes, then extracted in CH2Cl2. The organic phase was anhydrified over Na2SO4 and dried to give a residue which was taken up in petrolatum and filtered. The resultant solid was dried under vacuum at 40° C. to give 1.72 g of the title compound (yield: 89%).

WORKUP

后处理

  1. additionwas added
  2. temperaturerefluxed for 1 hour
  3. customdried
  4. additionadded with NaHCO3 up to alkalinity
  5. extractionextracted in CH2Cl2
  6. customdried
  7. customto give a residue which
  8. filtrationfiltered
  9. customThe resultant solid was dried under vacuum at 40° C.