HCID 10104631, compound → Ammonia

HRID 1180507Notes

Reaction equation

HRID 1180507 reaction equation
Cl[C:2]1[N:3]=[N:4][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:6][CH:7]=1>[Pd].C(O)C>[NH3:3].[N:3]1[CH:2]=[CH:7][CH:6]=[C:5]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[N:4]=1

Participants

5

Reactant 1

HCID 10104631HCID 10104631, compound

Product 2

HCID 222AmmoniaHCID 220534791-(pyridazin-3-yl)-1,4-diazepane

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 702EthanolSolvent

Procedure

A mixture of 1-(3-chloro-6-pyridazinyl)-homopiperazine (5.56 g, 26.1 mmol), palladium on carbon (2.1 g, 10%) and ethanol (150 ml) was stirred under hydrogen overnight. The crude product was filtered through celite and evaporated. Chromatography on silica gel with dichloromethane, methanol and conc. ammonia (89:10:1) gave the title compound as free base. Yield 2.78 g, 60%, 185.0-186.9° C.

Workup

  1. filtrationThe crude product was filtered through celite
  2. customevaporated

Sources & evidence

ORD record
ord-23663dc88f1845229b05d372bb5f7587
Source dataset
uspto-grants-2007_10
Patent number
US07282494B2

Reaction notes

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