2,3-Diaminopyridine → HCID 22732327, compound

HRID 2083983Notes

Reaction equation

HRID 2083983 reaction equation
[O:1]1[CH2:6][CH2:5][O:4][CH2:3][C:2]1=O.[NH2:8][C:9]1[C:14]([NH2:15])=[CH:13][CH:12]=[CH:11][N:10]=1>C1(C)C=C(C)C=C(C)C=1>[OH:1][CH2:6][CH2:5][O:4][CH2:3][C:2]1[NH:15][C:14]2[CH:13]=[CH:12][CH:11]=[N:10][C:9]=2[N:8]=1

Participants

4

Reactant 2

HCID 99562,3-DiaminopyridineHCID 18233Dioxanone

Product 1

HCID 22732327HCID 22732327, compound

Reagents, catalysts & solvents 1

HCID 7947MesityleneSolvent

Procedure

1,4-Dioxan-2-one (6.13 g, 60 mmol) and 2,3-diaminopyridine (5.46 g, 50 mmol) in mesitylene (100 ml) were heated at reflux in a Dean-Stark separator for 10 h. After cooling, mesitylene was decanted off and the residue was purified by silica gel chromatography (dichloromethane:methanol 9:1) (yield: 8.47 g, 87% of theory).

Workup

  1. temperatureat reflux in a Dean-Stark separator for 10 h
  2. temperatureAfter cooling
  3. custommesitylene was decanted off
  4. customthe residue was purified by silica gel chromatography (dichloromethane:methanol 9:1) (yield: 8.47 g, 87% of theory)

Sources & evidence

ORD record
ord-7c17a1e6421a40639efe41a7d6c02fed
Source dataset
uspto-grants-2004_04
Patent number
US06716849B1

Reaction notes

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