反应详情

In absolute anhydrous THF (15 mL) were dissolved N-benzyl-4-((3-chloro-4-methoxybenzyl)amino)-2-(methylsulfinyl)pyrimidine-5-formamide (180 mg, 0.41 mmol) and 5-azaspiro[2.4]heptane (59 mg, 0.61 mmol). The solution was cooled in an ice bath, and triethylamine (82 mg, 0.82 mmol) was added dropwisely. The reaction was conducted at ambient temperature for 8 h then was quenched with water. The reaction mixture was extracted with DCM. The organic phase was dried over sodium sulfate and concentrated. The obtained solid was purified by silica gel column chromatography (DCM/methanol=50/1) to give the product as a solid (35 mg, 18% yield).

1. temperatureThe solution was cooled in an ice bath
2. customthen was quenched with water
3. extractionThe reaction mixture was extracted with DCM
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated
6. customThe obtained solid was purified by silica gel column chromatography (DCM/methanol=50/1)