Nitric Acid → 1-Nitro-2,5-bis(trifluoromethyl)benzene

Temperatur

100 °C

1,4-Bis(trifluoromethyl)benzene (10.06 g, 47 mmol) in fuming sulfuric acid (20 g) was cooled to 0° C. Fuming nitric acid (8 g) was added cautiously. The mixture was heated to 100° C. and stirred for 1 hour. A mixture of fuming nitric acid (6 g) and fuming sulfuric acid (12 g) was added, and the mixture was heated to 110° C. and stirred for 6 hours. After cooling to r.t., the mixture was poured into ice water (150 g) cautiously, and extracted with chloroform (100 mL×3). The combined organic layers were washed with water (100 mL×2), 10% sodium hydroxide aqueous solution (100 mL×2), and then water (100 mL×2). The resulting organic layers were dried over sodium sulfate, filtered, and concentrated to afford 2-nitro-1,4-bis(trifluoromethyl)benzene as an oil (3.3 g).

1. additionwas added
2. temperaturethe mixture was heated to 110° C.
3. stirringstirred for 6 hours
4. temperatureAfter cooling to r.t.
5. extractionextracted with chloroform (100 mL×3)
6. washThe combined organic layers were washed with water (100 mL×2), 10% sodium hydroxide aqueous solution (100 mL×2)
7. dry with materialThe resulting organic layers were dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated

ORD-Eintrag

ord-891db7f645a64b44aeffa64ae7ae52b7

Quelldatensatz

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08969349B2