Hydrazine hydrate (1:1) → HCID 69656230, compound

HRID 1244795Notes

Reaction equation

HRID 1244795 reaction equation
C([O:4][CH2:5][C:6]12[O:26][C:13]3([CH2:18][CH2:17][N:16]([CH2:19][N:20]4[CH:25]=[CH:24][N:23]=[CH:22][CH2:21]4)[CH2:15][CH2:14]3)[CH2:12][CH:11]1[C:10](=[O:27])[CH2:9][CH:8]([C:28]([O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)=[O:29])[CH2:7]2)(=O)C.O.NN>C(O)C>[CH2:19]([N:16]1[CH2:17][CH2:18][C:13]2([CH2:12][CH:11]3[C:6]([CH2:5][OH:4])([CH2:7][CH:8]([C:28]([O:30][CH2:31][C:32]4[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=4)=[O:29])[CH2:9][C:10]3=[O:27])[O:26]2)[CH2:14][CH2:15]1)[N:20]1[CH:21]=[CH:22][N:23]=[CH:24][CH2:25]1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 69656390HCID 69656390, compound

Product 1

HCID 69656230HCID 69656230, compoundYield 89.6%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of the compound obtained in Step 5 (400 mg) in ethanol (8 ml) was added hydrazine monohydrate (0.38 ml) under cooling with ice. The mixture was stirred overnight at room temperature. The reaction mixture was concentrated and the resulting residue was purified by silica gel chromatography (eluent; methylene chloride:methanol=50:1–25:1) to obtain the title compound (329 mg).

Workup

  1. temperatureunder cooling with ice
  2. concentrationThe reaction mixture was concentrated
  3. customthe resulting residue was purified by silica gel chromatography (eluent; methylene chloride:methanol=50:1–25:1)

Sources & evidence

ORD record
ord-3af36f1e58184c09874679c9c7020865
Source dataset
uspto-grants-2006_10
Patent number
US07122662B2

Reaction notes

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