Ethanol → HCID 178470725, compound

HRID 547151Notes

Reaction equation

HRID 547151 reaction equation
S(=O)(=O)(O)O.[OH:6][C:7]1[CH:8]=[C:9]([CH2:14][C:15]([OH:17])=[O:16])[C:10](=[O:13])[NH:11][N:12]=1.[CH2:18](O)[CH3:19]>>[CH2:18]([O:16][C:15](=[O:17])[CH2:14][C:9]1[C:10](=[O:13])[NH:11][N:12]=[C:7]([OH:6])[CH:8]=1)[CH3:19]

Participants

4

Reactant 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 178525216HCID 178525216, compound

Product 1

HCID 178470725HCID 178470725, compoundYield 82%

Conditions

Temperature
88 °C

Procedure

Concentrated sulfuric acid (0.04 mL, 0.75 mmol) was added to a solution of (6-hydroxy-3-oxo-2,3-dihydro-pyridazin-4-yl)-acetic acid (Example 182-(1); 259 mg, 1.52 mmol) in ethanol (3.2 mL), and the mixture was heated while stirring at an external temperature of 84 to 92° C. for four hours. The mixture was left to stand at room temperature overnight. Then, the resulting solid was collected by filtration and sequentially washed with water and ether to give the title compound (246 mg, 82%).

Workup

  1. temperaturethe mixture was heated
  2. waitThe mixture was left
  3. waitto stand at room temperature overnight
  4. filtrationThen, the resulting solid was collected by filtration
  5. washsequentially washed with water and ether

Sources & evidence

ORD record
ord-bce3ae51f16141fe8534b736705ef1ae
Source dataset
uspto-grants-2011_05
Patent number
US07935688B2

Reaction notes

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