Sodium Hydroxide → HCID 18960804, compound

HRID 1084329Notes

Reaction equation

HRID 1084329 reaction equation
Br[C:2]1[C:3]([C:11]([OH:13])=[O:12])=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[N:6][CH:7]=1.[OH-:14].[Na+]>S([O-])([O-])(=O)=O.[Cu+2]>[OH:14][C:2]1[C:3]([C:11]([OH:13])=[O:12])=[CH:4][C:5]([C:8]([OH:10])=[O:9])=[N:6][CH:7]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 14256373HCID 14256373, compound

Product 1

HCID 18960804HCID 18960804, compound

Reagents, catalysts & solvents 1

HCID 24462Copper SulfateCatalyst

Conditions

Temperature
165 °C

Procedure

A mixture of 500 mg of 5-bromo-2,4-pyridinedicarboxylic acid from Example 2, 20 ml of 10 N aqueous sodium hydroxide solution and 250 mg of copper sulfate is heated at 165° C. in an autoclave for 4 hours. After cooling, the copper salt is filtered off with suction, the pH is brought to 1 with concentrated hydrochloric acid and the solution is evaporated. The solid is heated in a little methanol, the salts are filtered off and the solution is left to stand at 0° C. for 20 hours. The solid which has precipitated out is separated off and dried.

Workup

  1. temperatureAfter cooling
  2. filtrationthe copper salt is filtered off with suction
  3. customthe solution is evaporated
  4. temperatureThe solid is heated in a little methanol
  5. filtrationthe salts are filtered off
  6. waitthe solution is left
  7. customThe solid which has precipitated out
  8. customis separated off
  9. customdried

Sources & evidence

ORD record
ord-ec08c1e86fed4071a55a6bf8b71ffcad
Source dataset
uspto-grants-1991_04
Patent number
US05004748

Reaction notes

Loading…