反应详情

0.50 mL (6.6 mmol) isopropanol are added to 289 mg (7.23 mmol) sodium hydride (60%) in 100 mL THF and the mixture is stirred for 30 min at rt. After that time, 2.0 g (6.0 mmol) 3,6-diiodo-pyridazine are added and the mixture is stirred for 14 h at rt and for 14 h at 50° C. After that time, the mixture is poured into water and extracted with EtOAc. The organic layer is washed with water (2×) and dried over sodium sulphate. The solvent is removed in vacuo and the residue is purified by column chromatography (silicia gel; heptane:EtOAc gradient 0 to 50%).

1. stirringthe mixture is stirred for 14 h at rt and for 14 h at 50° C
2. extractionextracted with EtOAc
3. washThe organic layer is washed with water (2×)
4. dry with materialdried over sodium sulphate
5. customThe solvent is removed in vacuo
6. customthe residue is purified by column chromatography (silicia gel; heptane:EtOAc gradient 0 to 50%)