1-Methylcyclopropene synthesis
- Product Name:1-Methylcyclopropene
- CAS Number:3100-04-7
- Molecular formula:C4H6
- Molecular Weight:54.09
563-47-3
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Yield:3100-04-7 92.6%
Reaction Conditions:
with sodium hydride in toluene at 20 - 30; for 2 h;Inert atmosphere;Reagent/catalyst;Temperature;Solvent;
Steps:
1
Clean and dry four bottles with nitrogen rinse for 30 minutes, after rinsing, 20 g of toluene and 3.9 g of NaH were added under nitrogen protection, the NaH is a 65% content of mineral oil-coated sodium hydride, in the nitrogen under the protection of temperature gradually increased to 20-25 ° C, a mixture of 9.1 grams of 3-chloro-2-methylpropylene and 10 grams of toluene was added dropwise for one second, and the reaction temperature was controlled at 25-30 ° C for two hours, gradually precipitate a large amount of light yellow 1-methylcyclopropene sodium salt.The separated 1 - methyl cyclopropene sodium salt filtration, the solvent can be recycled, then 10 ml toluene wash the filter cake, washing twice to remove the raw materials and the by-product.The application of the prepared 1-methylcyclopropene 7.1 g, yield is 92.6%, taking a small amount of 1 - methyl cyclopropene water decomposition collecting 1 - methyl cyclopropene, GC analysis, the content of 99.5%; the cost is low, the solvent through the simple distillation can be recovering solvent and reaction directly recycled raw materials, environmental protection.
References:
CN106928015,2017,A Location in patent:Paragraph 0022-0025
130894-83-6
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920-46-7
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