Calcium Carbonate → HCID 57319731, compound

Participants

Reaction Conditions

Reaction Steps

0.15 mole (41.3 g) of 3,5-diamino-2,4-dimethoxychlorobenzene dihydrochloride obtained in Example 3, followed by 30 ml of 10N sodium hydroxide was added to 200 ml of dioxane. The temperature was raised to the region of 80° C., and then 15 g of calcium carbonate were added. 43 g of β-chloroethyl chloroformate were then introduced with stirring. Upon completion of the addition, heating was maintained at 90° C. for 15 minutes. The inorganic salts were removed from the reaction mixture by filtration. The expected product crystallized slowly upon dilution of the reaction mixture with iced water. Recrystallized from 96° strength ethanol, it melted at 87° C.

Provenance & Evidence