HRID840550

反应详情

EQUATION

反应方程式

HRID 840550 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (0.21 g of an 80% dispersion in oil, 7.0 mmol) was added to a solution of 3-hydroxy-2-methylpyridine (0.88 g, 8.0 mmol) in DMF (15 ml). After 1.5 h at r.t. a solution of 6-chloropyridazine-3-carboxylic acid ethyl ester (Chem. Pharm. Bull. 1994, 42(2), 371) (1.0 g, 5.4 mmol) in DMF (10 ml) was added and the mixture was stirred for a further 1.5 h. The DMF was removed in vacuo and the residue partitioned between dil. aq. NaOH (50 ml) and CH2Cl2 (100 ml). After drying (Na2SO4) the organics were evaporated to give the title compound as an off-white solid (1.09 g, 78%).

WORKUP

后处理

  1. customThe DMF was removed in vacuo
  2. customthe residue partitioned between dil. aq. NaOH (50 ml) and CH2Cl2 (100 ml)
  3. dry with materialAfter drying (Na2SO4) the
  4. customorganics were evaporated