Acetic Acid → HCID 178432317, compound

HRID 2231257Notes

Reaction equation

HRID 2231257 reaction equation
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[C:9](O)(=O)[CH3:10].[OH-].[NH4+]>O>[CH3:9][C:10]1[NH:8][C:7]2[CH:6]=[CH:5][N:4]=[CH:3][C:2]=2[N:1]=1

Participants

5

Reactant 3

HCID 176Acetic AcidHCID 59183,4-DiaminopyridineHCID 14923Ammonium Hydroxide

Product 1

HCID 178432317HCID 178432317, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
125 °C

Procedure

A mixture of 5 g of 3,4-diaminopyridine, 3.9 ml of acetic acid and 50 ml of polyphosphoric acid was heated to 125° C. for 2 hours. The reaction mixture was poured into water and the pH adjusted to 8 with ammonium hydroxide. The product was extracted with methanol-chloroform (1:1) and the extracts dried over sodium sulfate and concentrated to dryness. Extraction of the residue with 50 ml of hot ethanol gave 3.98 g of product.

Workup

  1. extractionThe product was extracted with methanol-chloroform (1:1)
  2. dry with materialthe extracts dried over sodium sulfate
  3. concentrationconcentrated to dryness
  4. extractionExtraction of the residue with 50 ml of hot ethanol

Sources & evidence

ORD record
ord-043ba360bb1640b8995af7dfe837bd99
Source dataset
uspto-grants-1988_11
Patent number
US04782050

Reaction notes

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