反应详情

In absolute anhydrous THF (10 mL) was dissolved 4-((3-chloro-4-methoxybenzyl)amino)-2-(methylsulfinyl)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide (100 mg, 0.22 mmol). Triethylamine (0.22 g, 2.2 mmol) was added dropwisely, and 3-azabicyclo[3.1.0]hexan hydrochloride salt (42 mg, 0.35 mmol) was added. The reaction mixture was heated to reflux overnight. The solvent was removed by rotary evaporation, and water was added, followed by extraction with DCM. The organic phase was dried over sodium sulfate and purified by silica gel column chromatography (DCM/methanol=20/1 to 10/1) to give a solid. The solid was dissolved in methanol (0.05 mL), and hydrochloric acid (1 mol/L) was added. The solvent was removed to give 2-(3-azabicyclo[3.1.0]hexan-3-yl)-4-((3-chloro-4-methoxybenzyl)amino)-N-(pyrimidin-2-ylmethyl)pyrimidine-5-formamide hydrochloride (40 mg, 39% yield).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux overnight
3. customThe solvent was removed by rotary evaporation, and water
4. additionwas added
5. extractionfollowed by extraction with DCM
6. dry with materialThe organic phase was dried over sodium sulfate
7. custompurified by silica gel column chromatography (DCM/methanol=20/1 to 10/1)
8. customto give a solid
9. customThe solvent was removed