Chloroform → HCID 54162718, compound

HRID 903114Notes

Reaction equation

HRID 903114 reaction equation
[Na].[CH:2]([CH:4]([CH2:7][NH:8][CH:9]=[O:10])[C:5]#[N:6])=O.[Cl-].[CH3:12][NH2+:13][CH3:14].C(Cl)(Cl)Cl>O>[CH3:12][N:13]([CH:2]=[C:4]([CH2:7][NH:8][CH:9]=[O:10])[C:5]#[N:6])[CH3:14]

Participants

6

Reactant 4

HCID 6212ChloroformHCID 5360545SodiumHCID 12954980Dimethylazanium;chlorideHCID 21541183HCID 21541183, compound

Product 1

HCID 54162718HCID 54162718, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

98.6 parts of 75 percent pure sodium salt of α-formyl-β-formylaminopropionitrile and 81.5 parts of dimethylammonium chloride in 700 parts by volume of chloroform are refluxed for 1.5 hours, during which time 8.5 parts (theory: 9 parts) of water are eliminated. The mixture is filtered, the filtrate is concentrated to dryness and the product is recrystallized from methanol. 43.0 parts of α-dimethylaminomethylene-β-formylaminopropionitrile of melting point 90° C. are obtained.

Workup

  1. filtrationThe mixture is filtered
  2. concentrationthe filtrate is concentrated to dryness
  3. customthe product is recrystallized from methanol

Sources & evidence

ORD record
ord-7d52ea1f9309424cbc163c5db1abd9c3
Source dataset
uspto-grants-1980_10
Patent number
US04226799

Reaction notes

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