Propylamine → HCID 86723282, compound

HRID 1846060Notes

Reaction equation

HRID 1846060 reaction equation
Cl[C:2]1[N:3]=[N:4][CH:5]=[C:6]([Cl:9])[C:7]=1[NH2:8].[CH2:10]([NH2:13])[CH2:11][CH3:12]>>[Cl:9][C:6]1[C:7]([NH2:8])=[C:2]([NH:13][CH2:10][CH2:11][CH3:12])[N:3]=[N:4][CH:5]=1

Participants

3

Reactant 2

HCID 7852PropylamineHCID 64032013,5-Dichloro-1,4-dihydropyridazin-4-imine

Product 1

HCID 86723282HCID 86723282, compoundYield 35%

Conditions

Temperature
125 °C

Procedure

A mixture of 3,5-dichloro-4-aminopyridazine (Preparation 4, 2 g, 12.3 mmol) and 70% aqueous propylamine (8 mL) was heated at 125° C. in an autoclave vessel for 5 hours. The reaction mixture was cooled to room temperature and evaporated to dryness. The crude residue was purified by silica gel column chromatography eluting with CH2Cl2:MeOH 98:2 to afford the title compound as a brown solid in 35% yield, 800 mg.

Workup

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customevaporated to dryness
  3. customThe crude residue was purified by silica gel column chromatography
  4. washeluting with CH2Cl2:MeOH 98:2

Sources & evidence

ORD record
ord-79e8c16db516460d9871791c4fd977a0
Source dataset
uspto-grants-2015_02
Patent number
US08952008B2

Reaction notes

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