Hydrazine hydrate (1:1) → HCID 69314656, compound

HRID 1394045Notes

Reaction equation

HRID 1394045 reaction equation
[F:1][C:2]1[CH:3]=[C:4]([CH:26]=[CH:27][C:28]=1[F:29])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][CH2:14][N:15]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:8][CH2:7]1.O.NN>CCO>[F:1][C:2]1[CH:3]=[C:4]([CH:26]=[CH:27][C:28]=1[F:29])[O:5][CH:6]1[CH2:7][CH2:8][N:9]([CH2:12][CH2:13][CH2:14][NH2:15])[CH2:10][CH2:11]1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 69312114HCID 69312114, compound

Product 1

HCID 69314656HCID 69314656, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To the product of Example 3, Step (c) in EtOH (30 ml) was added hydrazine monohydrate (0.562 ml). The reaction was refluxed for 4 hrs and the solvent evaporated. Dichlorornethane (40 ml) was added and the solid by-product filtered. The organic residue was evaporated and the product purified by reverse phase HPLC {with a gradient eluent system [25% MeCN/NH4OAcaq (0.1%) to 95% MeCN//NH4OAcaq (0.1%)]} to give the sub-title compound as a solid (0.622 g).

Workup

  1. temperatureThe reaction was refluxed for 4 hrs
  2. customthe solvent evaporated
  3. additionDichlorornethane (40 ml) was added
  4. filtrationthe solid by-product filtered
  5. customThe organic residue was evaporated
  6. customthe product purified by reverse phase HPLC {with a gradient eluent system [25% MeCN/NH4OAcaq (0.1%) to 95% MeCN//NH4OAcaq (0.1%)]

Sources & evidence

ORD record
ord-7a3a968cff8c448fabc07b15cf42b532
Source dataset
uspto-grants-2008_03
Patent number
US07348341B2

Reaction notes

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