Ethanol → HCID 176525526, compound

HRID 1680200Notes

Reaction equation

HRID 1680200 reaction equation
[Na].[NH2:2][C:3]1[NH:8][C:7]([CH3:10])([CH3:9])[N:6]=[C:5](SC)[N:4]=1.[CH2:13]([OH:15])[CH3:14]>>[NH2:2][C:3]1[NH:8][C:7]([CH3:10])([CH3:9])[N:6]=[C:5]([O:15][CH2:13][CH3:14])[N:4]=1

Participants

4

Reactant 3

HCID 702EthanolHCID 5360545SodiumHCID 176525525HCID 176525525, compound

Product 1

HCID 176525526HCID 176525526, compound

Procedure

To a solution of sodium (2.3 g., 0.1 gr. atom) in absolute ethanol (100 ml.) is added 2-amino-3,4-dihydro-4,4-dimethyl-6-methylthio-1,3,5-triazine (3.4 g., 0.02 mole) and the mixture is heated at reflux for 18 hours. The ethanol is distilled at reduced pressure and the residue dissolved in water (100 ml.) and extracted with ethyl acetate (3×100 ml.) dried over potassium carbonate and evaporated in vacuo to give 1.3 g of 2-amino-3,4-dihydro-4,4-dimethyl-6-ethoxy-1,3,5-triazine which melts at 175°-8° C. after crystallization from acetonitrile.

Workup

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 18 hours
  3. distillationThe ethanol is distilled at reduced pressure
  4. dissolutionthe residue dissolved in water (100 ml.)
  5. extractionextracted with ethyl acetate (3×100 ml.)
  6. dry with materialdried over potassium carbonate
  7. customevaporated in vacuo

Sources & evidence

ORD record
ord-a9de244e615e40dab90f9f56749c40da
Source dataset
uspto-grants-1981_06
Patent number
US04272537

Reaction notes

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