Chloroacetonitrile → HCID 117729502, compound

HRID 2173472Notes

Reaction equation

HRID 2173472 reaction equation
[CH3:1][C:2]1[C:7]([CH3:8])=[N:6][NH:5][C:4](=[S:9])[C:3]=1[C:10]#[N:11].C([O-])(=O)C.[Na+].Cl[CH2:18][C:19]#[N:20]>C(O)C.CC(O)C>[NH2:11][C:10]1[C:3]2[C:2]([CH3:1])=[C:7]([CH3:8])[N:6]=[N:5][C:4]=2[S:9][C:18]=1[C:19]#[N:20]

Participants

6

Reactant 3

HCID 7856ChloroacetonitrileHCID 517045Sodium AcetateHCID 256489772,3-Dihydro-5,6-dimethyl-3-thioxo-4-pyridazinecarbonitrile

Product 1

HCID 117729502HCID 117729502, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 3776IsopropanolSolvent

Procedure

The 5,6,-dimethyl-3-thioxo-2,3-dihydropyridazine-4-carbonitrile (99 mg, 0.60 mmol) was stirred in ethanol (6.0 mL). Sodium acetate (50 mg, 0.60 mmol) and chloroacetonitrile (0.040 mL, 0.60 mmol) were added and the mixture was stirred at ambient temperature for 90 minutes. The mixture was then diluted with IPA, stirred for 15 minutes, and filtered. The solute was concentrated in vacuo, and the resulting solid was dried overnight at 60° C. in a vacuum oven to give the product. LC/MS: RT=0.38 min., m/z=205 [M+H]+.

Workup

  1. stirringstirred for 15 minutes
  2. filtrationfiltered
  3. concentrationThe solute was concentrated in vacuo
  4. customthe resulting solid was dried overnight at 60° C. in a vacuum oven
  5. customto give the product

Sources & evidence

ORD record
ord-bcb2fbd5ca604b6381446071b81a4b68
Source dataset
uspto-grants-2015_06
Patent number
US09056875B2

Reaction notes

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