Sodium → HCID 178493623, compound

HRID 973844Notes

Reaction equation

HRID 973844 reaction equation
[CH3:1][O-:2].[Na+].[Na].Cl[C:6]1[CH:11]=[C:10]([SH:12])[N:9]2[N:13]=[CH:14][N:15]=[C:8]2[N:7]=1>CO>[SH:12][C:10]1[N:9]2[N:13]=[CH:14][N:15]=[C:8]2[N:7]=[C:6]([O:2][CH3:1])[CH:11]=1

Participants

5

Reactant 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 178527722HCID 178527722, compound

Product 1

HCID 178493623HCID 178493623, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a sodium methoxide solution, prepared from 1.4 g of sodium and 50 ml of methanol, was added all at once the product obtained in Step 1 of Example 43 (4.6 g) under ice cooling. The mixture was refluxed for one hour, the solution was concentrated under reduced pressure, and the remaining yellow oil was dissolved in 50 ml water. The pH was adjusted to 1.0 with 1N hydrochloric acid, and the formed crystals were collected by filtration and washed with 30 ml ethanol, giving 1.7 g of the objective compound as faint yellow crystals.

Workup

  1. temperatureThe mixture was refluxed for one hour
  2. concentrationthe solution was concentrated under reduced pressure
  3. dissolutionthe remaining yellow oil was dissolved in 50 ml water
  4. filtrationthe formed crystals were collected by filtration
  5. washwashed with 30 ml ethanol

Sources & evidence

ORD record
ord-c22380320b4647399558b8210f5f4a75
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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