Acetonitrile → HCID 69264785, compound

HRID 898696Notes

Reaction equation

HRID 898696 reaction equation
[Cl:1][C:2]1N=[N:6][C:5]([CH2:8]CCl)=[C:4](CCC)[CH:3]=1.[C:14]([O-])([O-])=O.[K+].[K+].[CH2:20]([NH2:24])[CH:21]([CH3:23])[CH3:22].[CH3:25][C:26]#[N:27]>>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]1[N:6]=[N:27][C:26]([CH2:14][NH:24][CH2:20][CH:21]([CH3:23])[CH3:22])=[CH:25][CH:8]=1

Participants

5

Reactant 4

HCID 6342AcetonitrileHCID 6558IsobutylamineHCID 11430Potassium CarbonateHCID 85991334HCID 85991334, compound

Product 1

HCID 69264785HCID 69264785, compound

Procedure

To a solution of 6-chloro-3-chloroethyl-4-propyl-pyridazine (3.4 g, 16.58 mmol) in CH3CN (30 ml) is added K2CO3 (9.15 g, 66.3 mmol), isobutylamine (6.6 ml, 66.3 mmol) and the mixture is stirred at room temperature overnight. The solvent is removed in vacuo and to the residue is added water (60 ml) and EtOAc (60 ml). The layers are separated and the organic layer is washed with brine (20 ml) and dried (Na2SO4). Evaporation of the solvent provides a light yellow oil, which is used to next step without further purification.

Workup

  1. customThe solvent is removed in vacuo and to the residue
  2. additionis added water (60 ml) and EtOAc (60 ml)
  3. customThe layers are separated
  4. washthe organic layer is washed with brine (20 ml)
  5. dry with materialdried (Na2SO4)
  6. customEvaporation of the solvent
  7. customprovides a light yellow oil, which
  8. customis used to next step without further purification

Sources & evidence

ORD record
ord-098c2906f5714ba88d96cba1e513d450
Source dataset
uspto-grants-2008_04
Patent number
US07351826B2

Reaction notes

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