Iodine → (5-Iodo-pyridin-2-yl)-methyl-amine

HRID 1350676

Reaktionsgleichung

Reaktionsgleichung von HRID 1350676
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[I:9]I.C([O-])(O)=O.[Na+]>CC(O)=O.O>[I:9][C:6]1[CH:7]=[CH:8][C:3]([NH:2][CH3:1])=[N:4][CH:5]=1

Komponenten

6

Edukt 3

HCID 807IodineHCID 207272-Pyridinamine, N-methyl-HCID 516892Sodium Bicarbonate

Produkt 1

HCID 11253290(5-Iodo-pyridin-2-yl)-methyl-amineAusbeute 24,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

To a solution of 2-methylaminopyridine (Aldrich; 1.00 g, 9.25 mmol) in 10 mL of 1:1 HOAc and water was added 2.35 g (9.25 mmol) of I2. The resulting brown solution was heated to 80° C. for 3 h. After cooling to room temperature, the mixture was neutralized with saturated NaHCO3 and extracted with Et2O. The extract was washed with water and brine, dried with MgSO4, filtered, and concentrated to provide 540 mg of (5-iodo-pyridin-2-yl)-methyl-amine.

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with Et2O
  3. washThe extract was washed with water and brine
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-096fabc787d84b3ebc1428aa1af0c299
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07214802B2

Verknüpfte Notizen

Wird geladen…