Water → HCID 178470462, compound

HRID 658374Notes

Reaction equation

HRID 658374 reaction equation
[CH2:1]([O:3][C:4](=[O:26])[C:5]([NH2:25])=[N:6][NH:7][C:8]([C:10]1[CH:15]=[CH:14][N:13]=[CH:12][C:11]=1[NH:16][C:17]1[CH:22]=[CH:21][C:20]([I:23])=[CH:19][C:18]=1[F:24])=O)[CH3:2].O>N1C=CC=CC=1>[CH2:1]([O:3][C:4]([C:5]1[NH:25][C:8]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][C:11]=2[NH:16][C:17]2[CH:22]=[CH:21][C:20]([I:23])=[CH:19][C:18]=2[F:24])=[N:7][N:6]=1)=[O:26])[CH3:2]

Participants

4

Reactant 2

HCID 962WaterHCID 68852573HCID 68852573, compound

Product 1

HCID 178470462HCID 178470462, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

Amino-{[3-(2-fluoro-4-iodo-phenylamino)-pyridine-4-carbonyl]-hydrazono}-acetic acid ethyl ester (1.6 g, 3.4 mmo) in pyridine (10 mL) was stirred at 140° C. for 3 hrs. Cooled, poured into water, Extracted with EtOAc, Combined the organic layer, and washed with Brine, dried over MgSO4, filtered, removed off solvent, got crude product, which was subjected to silica gel column (Hex:EtOAc=1:1). Collected final product 1.02 g. [5.23 min, 454 (M+1)]

Workup

  1. temperatureCooled
  2. extractionExtracted with EtOAc
  3. washwashed with Brine
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customremoved off solvent
  7. customCollected final product 1.02 g
  8. custom[5.23 min, 454 (M+1)]

Sources & evidence

ORD record
ord-eec3d49f87894b96908442b5e62684f5
Source dataset
uspto-grants-2011_12
Patent number
US08076486B2

Reaction notes

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