Hydrazine hydrate (1:1) → HCID 14221745, compound

HRID 1619480Notes

Reaction equation

HRID 1619480 reaction equation
[CH2:1]([N:3]1[C:15]2[CH:14]=[N:13][C:12](C(OCC)=O)=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH3:2].O.NN>C(O)C>[CH2:1]([N:3]1[C:15]2[CH:14]=[N:13][CH:12]=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH3:2]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 14221744Ethyl 9-ethyl-9H-beta-carboline-3-carboxylate

Product 1

HCID 14221745HCID 14221745, compoundYield 101.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Compound 31 (2.7 g, 10 mmol) was dissolved into ethanol (50 ml). 85% Hydrazine hydrate (15 ml) was added. The mixture was refluxed by heating for 6 h and concentrated to 30 ml in reduced pressure. After cooling, filtration, wash with ethanol, and natural drying in the air, white solids (2.0 g, 83%) were obtained. Samples for analysis could be recrystallized by 90% ethanol to obtain white flaring sheet-like crystals, mp 195-196° C.

Workup

  1. temperatureThe mixture was refluxed
  2. temperatureby heating for 6 h
  3. concentrationconcentrated to 30 ml in reduced pressure
  4. temperatureAfter cooling
  5. filtrationfiltration
  6. washwash with ethanol
  7. customnatural drying in the air

Sources & evidence

ORD record
ord-449c4fe3368c49b68a17ba002e6ee7f6
Source dataset
uspto-grants-2014_07
Patent number
US08772311B2

Reaction notes

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