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In a 2 liter-volume four-necked flask having the same equipments as used in 1) above were charged 100 g of 1,4-bis(1,2-dibromoethyl)benzene, 103 g of potassium t-butoxide and 1 liter of t-butyl alcohol, and the mixture was stirred taking care not to rapidly raise the temperature by cooling on an ice bath. The stirring was continued while gradually elevating the temperature finally to a refluxing temperature, at which stirring was conducted for 1.5 hours. The reaction mixture was poured into 6 liters of ice-water, and the thus formed precipitate was filtered by suction. Purification by sublimation (60°±3° C., 1 to 2 mmHg) gave 22.4 g of crystals of p-diethynylbenzene ##STR8## having a melting point of 96.5° C.

1. temperatureto rapidly raise the temperature
2. temperatureby cooling on an ice bath
3. stirringat which stirring
4. filtrationthe thus formed precipitate was filtered by suction
5. customPurification by sublimation (60°±3° C., 1 to 2 mmHg)