Reaktion #47936

ord-c55d733421a444529c3510bfaeac415c

Reaktionsgleichung

O=S(=O)([O-])O.[K+]
KHSO4
Oc1ccnc(O)c1
2,4-dihydroxypyridine
O=C([O-])[O-].[K+].[K+]
K2CO3
II
I2
Oc1ccnc(O)c1I
2,4-dihydroxy-3-iodopyridine

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGWith continued stirring
  2. 2
    Temperaturheating
  3. 3
    SonstigeWhen the solid I2 was consumed
  4. 4
    Temperaturthe mixture was cooled
  5. 5
    FiltrationThe precipitate was collected by filtration
  6. 6
    Waschenrinsed with water

Vorschrift

A mixture of 2,4-dihydroxypyridine (1.0 eq), K2CO3 (1.0 eq), and water was stirred at 100° C. so that it became homogeneous. With continued stirring and heating, I2 (1.0 eq) was added in portions, causing the evolution of gas. When the solid I2 was consumed, the mixture was cooled and acidified with aqueous KHSO4 (1.0 eq), generating a precipitate. The precipitate was collected by filtration, rinsed with water, and stored under high vacuum, to give 2,4-dihydroxy-3-iodopyridine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745454B2uspto-grants-2010_06