Preparation of Cyanamide
Typical Procedure:Glacial acetic acid 57 g (54 mL, 0.75 mol) and water 135 mL are placed in a large sized agate mortar and white thoroughly stirring, calcium cyanamide 40 g (0.50 mol) is slowly added and the mixture is grounded. Acetylene gas is generated, yielding a dull grayish to dark colored paste. Subsequently, the paste is dried at 40~50 ℃ for 12~18 hours under reduced pressure 30 mmHg to yield a gray powder which is placed in a Soxhlet extractor. The powder is extracted with 400 mL of ether containing several drops of dilute acetic acid for 2~3 hours (2×). The ether extraction is dried over anhydrous sodium sulfate (30 g). Concentration under a reduced pressure gives 10.5~15.8 g (50~75% from CaCN2) colorless viscous oil.
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Org. Synth. 1963, Coll. Vol. 4, 645.