Sodium Acetate → 4-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

HRID 1110111Notes

Reaction equation

HRID 1110111 reaction equation
C([NH:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12])(=O)C.C([O-])(=O)C.[Na+]>Cl>[NH2:4][N:5]1[CH2:10][C:9]([CH3:11])=[N:8][NH:7][C:6]1=[O:12]

Participants

4

Reactant 2

HCID 517045Sodium AcetateHCID 11008343N-(6-Methyl-3-oxo-2,5-dihydro-1,2,4-triazin-4(3H)-yl)acetamide

Product 1

HCID 109755004-Amino-6-methyl-2,5-dihydro-1,2,4-triazin-3-one

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
80 °C

Procedure

A mixture of 1.7 g of 4-acetylamino-6-methyl-3-oxo-2,3,4,5-tetrahydro-1,2,4-triazine and 10 ml of 2N hydrochloric acid is stirred for 5 hours at 80° C. After cooling, 1.7 g of sodium acetate are added, and the mixture is concentrated by evaporation in vacuo at a bath temperature of 60° C. The residue is taken up in ethanol, and salt precipitates are filtered off. The filtrate is concentrated to a small volume and caused to crystallise. The title compound is obtained in the form of colourless crystals having a melting point of 116°-119° C.

Workup

  1. temperatureAfter cooling
  2. concentrationthe mixture is concentrated by evaporation in vacuo at a bath temperature of 60° C
  3. customsalt precipitates
  4. filtrationare filtered off
  5. concentrationThe filtrate is concentrated to a small volume
  6. customto crystallise

Sources & evidence

ORD record
ord-beab8bbf88c3413cbc5e3a557d293915
Source dataset
uspto-grants-1994_06
Patent number
US05324842

Reaction notes

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