Bromine → 3-Bromo-6-(trifluoromethyl)pyridin-2-amine

HRID 451465

Reaktionsgleichung

Reaktionsgleichung von HRID 451465
[F:1][C:2]([F:11])([F:10])[C:3]1[N:8]=[C:7]([NH2:9])[CH:6]=[CH:5][CH:4]=1.[Br:12]Br>ClCCl>[Br:12][C:6]1[C:7]([NH2:9])=[N:8][C:3]([C:2]([F:1])([F:10])[F:11])=[CH:4][CH:5]=1

Komponenten

4

Edukt 2

HCID 24408BromineHCID 8210242-Amino-6-(trifluoromethyl)pyridine

Produkt 1

HCID 547588353-Bromo-6-(trifluoromethyl)pyridin-2-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 6-(trifluoromethyl)pyridin-2-amine (200 mg, 1.23 mmol) in dichlormethane (2.47 mL) was cooled to 0° C. and bromine (197 mg, 63.4 μL, 1.23 mmol) was slowly added within 30 minutes. After 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine, dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography over silica gel using CH2Cl2/MeOH (with 10% ammonia) as eluent. The title compound was obtained as a white solid (711 mg, 24%).

Aufarbeitung

  1. extractionAfter 25 hours at 0° C. the reaction mixture was extracted with saturated Na2S2O3 solution, water and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe crude material was purified by flash chromatography over silica gel

Quellen und Nachweise

ORD-Eintrag
ord-f55ec016212748739785ce7fd3b023d5
Quelldatensatz
uspto-grants-2013_07
Patentnummer
US08486967B2

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