Hydrazine → HCID 13533700, compound

HRID 465108Notes

Reaction equation

HRID 465108 reaction equation
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:5]=[CH:4][CH:3]=1.[NH2:14][NH2:15]>N1C=CC=CC=1>[NH:14]([C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][N:9]=2)[CH:5]=[CH:4][CH:3]=1)[NH2:15]

Participants

4

Reactant 2

HCID 9321Hydrazine3×HCID 111168506-CHLORO-2,2'-BIPYRIDINE

Product 1

HCID 13533700HCID 13533700, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A mixture of 4.0 g of 6'-chloro-2,2'-bipyridine and 10 ml of anhydrous hydrazine in 50 ml of dry pyridine was refluxed for 48 hours. Additional hydrazine (10 ml) was added and the solution was refluxed for an additional 72 hours while 5 ml portions of hydrazine were added at 18 hour intervals. The volatiles were removed under vacuum, the residue dissolved in ether, dried over sodium sulfate and concentrated to a solid. This solid was recrystallized from ether-heptane, giving 3.0 g of 6'-hydrazino-2,2'-bipyridine as white crystals, mp 69°-70° C.

Workup

  1. temperaturewas refluxed for 48 hours
  2. additionwere added at 18 hour intervals
  3. customThe volatiles were removed under vacuum
  4. dissolutionthe residue dissolved in ether
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated to a solid
  7. customThis solid was recrystallized from ether-heptane

Sources & evidence

ORD record
ord-715397ce801848ceafd87c4b5540ba5e
Source dataset
uspto-grants-1985_10
Patent number
US04550166

Reaction notes

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