Calcium Carbonate → HCID 19878616, compound

HRID 1885490Notes

Reaction equation

HRID 1885490 reaction equation
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[CH:4][N:3]=1.[C:9](=[O:12])([O-:11])[O-].[Ca+2].[CH2:14]([O:16][C:17](Cl)=[O:18])[CH3:15].O1CCO[CH2:22][CH2:21]1>>[CH2:21]([O:11][C:9]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:17]([O:16][CH2:14][CH3:15])=[O:18])=[CH:4][N:3]=1)=[O:12])[CH3:22]

Participants

5

Reactant 4

HCID 10112Calcium Carbonate2×HCID 10928Ethyl chloroformateHCID 203142,5-PyridinediamineHCID 312751,4-Dioxane2×

Product 1

HCID 19878616HCID 19878616, compound

Procedure

10 g of 2,5-diamino-pyridine are suspended together with 20 g of calcium carbonate in 100 ml of dioxane while stirring and heated to 70° C., whereupon 20 ml of chloroformic ethyl ester are slowly added dropwise and stirring is continued over night at 70° C. Subsequently while rewashing with dioxane some of the excess calcium carbonate is filtered with suction while still hot and the filtrate is concentrated in vacuo. The residue crystallizes from ethanolic solution. The compound can also be produced according to H. Meyer and F. Staffen, Monatsch. Chemie 34, Page 517 ff. (1913).

Workup

  1. additionare slowly added dropwise
  2. stirringstirring
  3. waitis continued over night at 70° C
  4. filtrationis filtered with suction while still hot and the filtrate
  5. concentrationis concentrated in vacuo
  6. customThe residue crystallizes from ethanolic solution
  7. customThe compound can also be produced

Sources & evidence

ORD record
ord-0ae3e2238a3c4e32b08e259914663182
Source dataset
uspto-grants-1992_09
Patent number
US05145482

Reaction notes

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