Diethyl Ether → HCID 178518690, compound

HRID 2214444Notes

Reaction equation

HRID 2214444 reaction equation
[NH2:1][C:2]1[C:3]([OH:9])=[N:4][CH:5]=[CH:6][C:7]=1[NH2:8].[K].CCO[C:14](S)=[S:15].C(OCC)C>C(O)C>[SH:15][C:14]1[NH:1][C:2]2[C:3](=[O:9])[NH:4][CH:5]=[CH:6][C:7]=2[N:8]=1

Participants

5

Reactant 3

HCID 3283Diethyl EtherHCID 45051758140-89-6HCID 178507904HCID 178507904, compound

Product 1

HCID 178518690HCID 178518690, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A suspension of 5.0 g (39.96 mmol) of 3,4-diamino-2-hydroxypyridine and 12.82 g (80.0 mmol) of potassium-ethyl xanthogenate in 100 ml of ethanol was refluxed for three hours. The mixture was then cooled to ambient temperature and combined with approx. 20 ml of diethyl ether. The precipitated product was filtered off, washed with approx. 10 ml of diethyl ether, dried, dissolved in approx. 30 ml of water and this solution was acidified with concentrated hydrochloric acid. The product precipitated was suction filtered, washed with 15 ml of water and dried at 50° C.

Workup

  1. temperaturewas refluxed for three hours
  2. filtrationThe precipitated product was filtered off
  3. washwashed with approx. 10 ml of diethyl ether
  4. customdried
  5. dissolutiondissolved in approx. 30 ml of water
  6. customThe product precipitated
  7. filtrationfiltered
  8. washwashed with 15 ml of water
  9. customdried at 50° C.

Sources & evidence

ORD record
ord-0d74910694d74a2095f7fab5f1700be2
Source dataset
uspto-grants-2006_09
Patent number
US07109192B2

Reaction notes

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