1-Heptyne synthesis
- Product Name:1-Heptyne
- CAS Number:628-71-7
- Molecular formula:C7H12
- Molecular Weight:96.17
Yield:628-71-7 80%
Reaction Conditions:
with ammonia;sodium at -40 - 20;
Steps:
1 Example 1
In a fume hood, a 3L three-necked flask was placed in a cold bath at -40° C, and ammonia gas was passed through for 1 hour to obtain a 1 L liquid ammonia solution. Subsequently, acetylene gas was continuously fed into the flask, and metallic sodium (46.0 g, 2.0 mol) was cut into small pieces, which were slowly added to the solution piece by piece, and the whole process was continued for 1 hour. Finally, 1-bromo-n-pentane (302.1 g, 2.0 mol) was added dropwise to the flask, and the addition was completed within 1 to 2 hours. After the addition was completed, the cooling bath was removed, the reaction flask was slowly warmed to room temperature, and 200 mL of concentrated aqueous ammonia was added to quench the reaction. The resulting mixture was separated and the organic phase was washed successively with dilute hydrochloric acid, saturated aqueous sodium carbonate solution and saturated brine. The organic phase was dried over anhydrous sodium sulfate and then distilled to give 1-heptyne (153.9 g, purity 97%, yield 80%).
References:
Wanhua Chemical Group Co., Ltd.;Huang Wenxue;Zhang Yongzhen;Li Wenbin;Wang Wen;Yu Bincheng;Li Yuan CN107805201, 2018, A Location in patent:Paragraph 0026; 0053; 0054
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