Cyclohexylmethyl bromide synthesis
- Product Name:Cyclohexylmethyl bromide
- CAS Number:2550-36-9
- Molecular formula:C7H13Br
- Molecular Weight:177.08
3725-11-9
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2550-36-9
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Yield:2550-36-9 90.3%
Reaction Conditions:
with 15-crown-5;sodium bromide at 20 - 80;Temperature;Reagent/catalyst;
Steps:
3 Example 3
200 g of cyclohexylmethanol and 222.6 g of sodium carbonate were added to 1 L of toluene, stirred and cooled to 10-20 C.At this temperature, 515 g of p-toluenesulfonyl chloride (dissolved in 2L of toluene) was added dropwise over 2.5 hours. After the dropwise addition, the amount was increased to 30.Esterification at ~35°C until the cyclohexane methanol GC content is 3% and filtration to obtain the organic phase intermediate filtrate, intermediate the organic phaseThe body filtrate was transferred to a 5L four-necked flask equipped with a magnetic stirrer, and 344 g of sodium bromide was added thereto while stirring at 20-35°C.15-crown-5catalyst 10g, after the completion of the addition, the temperature was raised to 70-80°C, and the reaction was incubated until the organic phase intermediate GC content was 3.6%.At 40°C, the organic phase filtrate is filtered and recovered. Distillation of toluene is performed and distillation is performed to obtain a pale yellow transparent product. The pale yellow transparent product is dried.After the product (bromomethyl)cyclohexane140.2 g, GC content 98%, yield 90.3%.
References:
Changzhou Woteng Chemical Technology Co., Ltd.;Sun Bo;Liu Zuhe;Yao Yuan;Xie Rong CN107652162, 2018, A Location in patent:Paragraph 0010-0013
100-49-2
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2550-36-9
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931-50-0
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2550-36-9
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108-85-0
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2550-36-9
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2043-61-0
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2550-36-9
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