Chloroacetonitrile → HCID 117729502, Verbindung

HRID 2173472Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2173472
[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]

Komponenten

6

Edukt 3

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

Produkt 1

HCID 117729502HCID 117729502, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

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]+.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-bcb2fbd5ca604b6381446071b81a4b68
Quelldatensatz
uspto-grants-2015_06
Patentnummer
US09056875B2

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