反应详情

Sodium hydride (10 mg, 0.24 mmol) was added to a solution of 4-{N-(6-Chloro-3-pyridazinyl)-5-aminopentan-1-oxy}benzaldehyde (51 mg, 0.16 mmol) in THF (3.5 ml) and the mixture was stirred at room temperature for 30 minutes. Methyl iodide (50 μl, 0.8 mmol) was added to the reaction mixture and the suspension was stirred at room temperature for 48 hours. The reaction mixture was poured into water (1.5 ml) and concentrated under reduced pressure. The residue was partitioned between water (2 ml) and ethyl acetate (40 ml), shaken thoroughly and the organic layer was separated, dried and evaporated to give a yellow solid. Purification by chromatography on silica gel (6 g, 30% ethyl acetate/hexane) gave 4-{N-(6-Chloro-3-pyridazinyl)-N-methyl-5-aminopentan-1-oxy}benzaldehyde (16 mg, 30%) as a pale yellow oil.

1. stirringthe suspension was stirred at room temperature for 48 hours
2. concentrationconcentrated under reduced pressure
3. customThe residue was partitioned between water (2 ml) and ethyl acetate (40 ml)
4. stirringshaken thoroughly
5. customthe organic layer was separated
6. customdried
7. customevaporated
8. customto give a yellow solid
9. customPurification by chromatography on silica gel (6 g, 30% ethyl acetate/hexane)