Acetic Acid → HCID 22346771、化合物

Under an argon atmosphere, 2-chloropyrimidine (2.68 g) and acetic acid (1.97 ml) were added to a solution of 4-bromoaniline (4.03 g) in dioxane (200 ml), and the resulting mixture was stirred for 3 hours while heating the mixture to reflux. Saturated aqueous sodium hydrogen carbonate solution was added in small portions to the reaction solution to neutralize it, and the resulting mixture was concentrated. Ethyl acetate (500 ml) was added to the residue and the resulting mixture was stirred at room temperature for 10 minutes, followed by removing insoluble matter by filtration. The filtrate was washed with saturated aqueous sodium hydrogen carbonate solution and with saturated brine, and dried over anhydrous sodium sulfate. After removing anhydrous sodium sulfate by filtration, the filtrate was concentrated. The residue was recrystallized from ethyl acetate to obtain N-(4-bromophenyl)pyrimidin-2-amine (3.02 g).

1. temperaturewhile heating the mixture
2. temperatureto reflux
3. concentrationthe resulting mixture was concentrated
4. additionEthyl acetate (500 ml) was added to the residue
5. stirringthe resulting mixture was stirred at room temperature for 10 minutes
6. customby removing insoluble matter
7. filtrationby filtration
8. washThe filtrate was washed with saturated aqueous sodium hydrogen carbonate solution and with saturated brine
9. dry with materialdried over anhydrous sodium sulfate
10. customAfter removing anhydrous sodium sulfate
11. filtrationby filtration
12. concentrationthe filtrate was concentrated
13. customThe residue was recrystallized from ethyl acetate

ORDレコード

ord-9f19905a0c6e43a8baee8a2d5a6fca51

出典データセット

uspto-grants-2009_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07566724B2