Acetic Acid → N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridine-2,3-diamine

온도

70 °C

A mixture of an iron powder (2.12 g), ethanol 6 ml), water 4 ml) and acetic acid 0.1 ml) was added dropwise a mixture of (3-nitro-5-trifluoromethylpyridin-2-yl)-(2,2,2-trifluoroethyl)amine (1.83 g) and ethanol (10 ml) at 70° C., and then the mixture was stirred at 70° C. for 1 hour. After allowing to cool, the cooled reaction mixture was filtrated. To the filtrate was added water, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate, and concentrated under reduced pressure to give N2-(2,2,2-trifluoroethyl)-5-trifluoromethylpyridin-2,3-diamine (1.59 g).

1. additionwas added dropwise
2. temperatureto cool
3. customthe cooled reaction mixture
4. filtrationwas filtrated
5. additionTo the filtrate was added water
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated under reduced pressure

ORD 기록

ord-12e41fe0f68845928d4e53325513b789

출처 데이터셋

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09403771B2