Butyl iodide → HCID 57762530、化合物

Under an argon atmosphere, N-(4-bromophenyl)pyrimidin-2-amine (160 mg) was added to a suspension of sodium hydride (33 mg) in anhydrous DMF (3 ml), and the resulting mixture was stirred at room temperature for 30 minutes. The reaction solution was cooled to 0° C. and n-butyl iodide (0.080 ml) was added thereto, followed by stirring the resulting mixture at room temperature for 1 hour, Saturated brine was added to the reaction solution and the resulting mixture was extracted 3 times with ethyl acetate. Organic layers were washed 3 times with water and once with saturated brine, and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated. The residue was purified by column chromatography (silica gel, eluent: ethyl acetate/hexane=1/10) to obtain N-(4-bromophenyl)-N-butylpyrimidin-2-amine (194 mg).

1. temperatureThe reaction solution was cooled to 0° C.
2. stirringby stirring the resulting mixture at room temperature for 1 hour
3. extractionthe resulting mixture was extracted 3 times with ethyl acetate
4. washOrganic layers were washed 3 times with water
5. dry with materialonce with saturated brine, and dried over anhydrous sodium sulfate
6. customAfter removing anhydrous sodium sulfate
7. filtrationby filtration
8. concentrationthe filtrate was concentrated
9. customThe residue was purified by column chromatography (silica gel, eluent: ethyl acetate/hexane=1/10)

ORDレコード

ord-4aa3a00e050847238a6b1e43661058be

出典データセット

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09162988B2