Calcium Carbonate → HCID 19878616, compound

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

Reactant 4

HCID 10112Calcium Carbonate2×

HCID 10928Ethyl chloroformate

HCID 203142,5-Pyridinediamine

HCID 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).