Methanol → HCID 178511136, compound

HRID 1075778Notes

Reaction equation

HRID 1075778 reaction equation
[CH3:1][OH:2].[CH3:3][O-:4].[Na+:5].[C]=O.[NH2:8][CH2:9][CH2:10][C:11]#[N:12]>C(OCC)=O>[Na:5][C:1]([CH:10]([CH2:9][NH:8][CH:3]=[O:4])[C:11]#[N:12])=[O:2]

Participants

6

Reactant 4

HCID 887MethanolHCID 16473-AminopropionitrileHCID 10942334Sodium MethoxideHCID 178418416HCID 178418416, compound

Product 1

HCID 178511136HCID 178511136, compoundYield 94%

Reagents, catalysts & solvents 1

HCID 8025Ethyl formateSolvent

Conditions

Temperature
25 °C

Procedure

In 400 parts by volume of ethyl formate is dissolved 35 parts of β-aminopropionitrile. To the solution is added 100 parts of a methanol solution which includes 32 parts of sodium methylate. The mixture is put into an autoclave with a capacity of 1,000 parts by volume. Into the mixture is introduced carbon monoxide at 50 kg/cm2G at 70°C for 3 hours. After the reaction, the mixture is cooled at 25°C. The solvent is removed and the crystals are recovered by filtration and dried, whereby 77 parts of α-sodioformyl-β-formylaminopropionitrile is obtained as crude crystals. Purity; 90 %. Yield: 94 %. Melting point; 190°C.

Workup

  1. customAfter the reaction
  2. customThe solvent is removed
  3. filtrationthe crystals are recovered by filtration
  4. customdried

Sources & evidence

ORD record
ord-b2489a3051a44ec3b0fc2b5f7e4afc42
Source dataset
uspto-grants-1976_05
Patent number
US03954756

Reaction notes

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