Реакция #418012

Уравнение реакции

water

isopropanol

sodium hydride

3,6-diiodo-pyridazine

→

3-Iodo-6-isopropoxy-pyridazine

Растворители

THF

Условия реакции

Обработка

1. 1
   workup.STIRRINGthe mixture is stirred for 14 h at rt and for 14 h at 50° C
2. 2
   Экстракцияextracted with EtOAc
3. 3
   ПромывкаThe organic layer is washed with water (2×)
4. 4
   Сушкаdried over sodium sulphate
5. 5
   ДругоеThe solvent is removed in vacuo
6. 6
   Другоеthe residue is purified by column chromatography (silicia gel; heptane:EtOAc gradient 0 to 50%)

Методика

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%).

Источник