Cyclopropylacetylene synthesis
- Product Name:Cyclopropylacetylene
- CAS Number:6746-94-7
- Molecular formula:C5H6
- Molecular Weight:66.1
Similarly, cyclopropylacetylene has been prepared by base-induced dehydrohalogenation of bromovinylcyclopropane . Cyclopropylacetylene has also been prepared from the 1-trimethylsilyl derivative of cyclopropylacetylene, which was prepared by treatment of 5-chloro-1-trimethylsilyl-1-pentyne with lithium diisopropylamide at ?78°C followed by warming to room temperature.
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Yield:6746-94-7 102.2 g
Reaction Conditions:
Stage #1:Cyclopropyl methyl ketone with triphenyl phosphite;bromine;triethylamine in dichloromethane at -10; for 2 h;Reflux;Green chemistry;
Stage #2: with potassium hydroxide in dimethyl sulfoxide at 40 - 110; for 2 h;Green chemistry;Reagent/catalyst;Solvent;
Steps:
1; 2; 3; 4; 5 [Example 3] Preparation of bromoethylene cyclopropane
Put 1.8 mol of cyclopropyl methyl ketone, 1.9 mol of triphenyl phosphite, 1.9 mol of triethylamine and 800 ml of dichloromethane into a 5L four-neck reaction flask, control the temperature -1010, and add 1.9 mol of liquid bromine dropwise After 2 hours, the dropwise addition was completed, the reaction was 2-4 hours, and the reflux was 1-3 hours. GC detected the reaction of cyclopropyl methyl ketone.After the reaction was completed, it was lowered to room temperature and filtered. The filter cake was added with aqueous sodium hydroxide solution and extracted with methylene chloride.The filtrate was evaporated under normal pressure to dry the solvent methylene chloride. The product was collected under reduced pressure 239g, the main product purity was 84.3%, the by-product isomer was 12.1%, and the yield of the product bromoethylene cyclopropane was 90.3%.[Example 4] Preparation of cyclopropylacetylenePut 1.795mol potassium hydroxide and 131 dimethyl sulfoxide into a 1L four-neck reaction flask, raise the temperature to 40-110, add 239g (1.63mol) of one-step product dropwise, complete the reaction for 2h, GC detection reaction is completed, filter, The filtrate was distilled to obtain 102.2 g of cyclopropylacetylene with a purity of 99% and a yield of 95%.
References:
Zhonghao (Dalian) Chemical Design Yuan Co., Ltd.;Wang Kewei;Liu Wei;Tang Peikun;Zhao Wenwu;Cai Xiaochuan;Dong Wuqing;Xu Han;Han Jianguo CN111116284, 2020, A Location in patent:Paragraph 0028-0032
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