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Bromine → 6-Bromo-2,4-dimethylpyridin-3-amine

HRID 1811585
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1811585
[CH3:1][C:2]1[C:7]([NH2:8])=[C:6]([CH3:9])[CH:5]=[CH:4][N:3]=1.[Br:10]Br>C(Cl)Cl>[Br:10][C:4]1[N:3]=[C:2]([CH3:1])[C:7]([NH2:8])=[C:6]([CH3:9])[CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24408BromineHCID 149107812,4-Dimethylpyridin-3-amine

Produkt 1

HCID 288753476-Bromo-2,4-dimethylpyridin-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 2,4-dimethylpyridin-3-amine (2.0 g, 16 mmol) in CH2Cl2 (20 mL), was added a solution of bromine (3.16 g; 20 mmol) in CH2Cl2 (5 mL) at 0° C. for 5 min. The reaction was concentrated under vacuum. The reaction was poured into H2O (50 mL), extracted with CH2Cl2, washed with Na2SO3 solution, and dried over MgSO4. The CH2Cl2 was concentrated under vacuum to afford the crude compound. The crude was purified over SiO2 to afford to give 6-bromo-2,4-dimethylpyridin-3-amine. 1HNMR (CDCl3, 400 MHz) δ 2.10 (s, 3H), 2.31 (s, 3H), 4.85-5.10 (b, 2H), 7.05 (s, 1H). Exact mass calculated for C7H9BrN2 201.06. found 202.3 (MH+).

Aufarbeitung

  1. concentrationThe reaction was concentrated under vacuum
  2. additionThe reaction was poured into H2O (50 mL)
  3. extractionextracted with CH2Cl2
  4. washwashed with Na2SO3 solution
  5. dry with materialdried over MgSO4
  6. concentrationThe CH2Cl2 was concentrated under vacuum
  7. customto afford the crude compound
  8. customThe crude was purified over SiO2
  9. customto afford

Quellen und Nachweise

ORD-Eintrag
ord-2c4a5becfc7546ecb8a27cf100868a25
Quelldatensatz
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08362248B2

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