Hydrochloric Acid → HCID 178470723, compound

HRID 973820Notes

Reaction equation

HRID 973820 reaction equation
[NH2:1][C:2]1[N:6]=[CH:5][NH:4][N:3]=1.[CH3:7][CH2:8][O:9][C:10]([CH2:12][C:13]([CH2:15][C:16](OCC)=[O:17])=O)=[O:11].Cl>C(O)(=O)C>[CH2:8]([O:9][C:10]([CH2:12][C:13]1[CH:15]=[C:16]([OH:17])[N:3]2[N:4]=[CH:5][N:6]=[C:2]2[N:1]=1)=[O:11])[CH3:7]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 66045Diethyl acetonedicarboxylateHCID 178418311HCID 178418311, compound

Product 1

HCID 178470723HCID 178470723, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A suspension of 3-amino-s-triazole (28 g) and diethyl acetonedicarboxylate (100 g) in 100 ml of acetic acid was refluxed for six hours. After cooling to room temperature, 150 ml of concentrated hydrochloric acid was added under ice cooling, the crystals thus formed were collected by filtration, and washed twice with 100 ml of ethanol, then once with 100 ml of ether, affording 71 g of the objective compound as colorless crystals.

Workup

  1. temperaturewas refluxed for six hours
  2. customthe crystals thus formed
  3. filtrationwere collected by filtration
  4. washwashed twice with 100 ml of ethanol

Sources & evidence

ORD record
ord-b0fae8d6e948494aa95160467f5738c0
Source dataset
uspto-grants-1991_11
Patent number
US05064953

Reaction notes

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