ChemicalBook CAS DataBase List 4-Methoxycyclohexanon

4-Methoxycyclohexanon synthesis

12synthesis methods

Product Name:4-Methoxycyclohexanon
CAS Number:13482-23-0
Molecular formula:C7H12O2
Molecular Weight:128.17

150-76-5

13482-23-0

The general procedure for the synthesis of p-methoxycyclohexanone from p-hydroxyanisole is as follows: 7 g of palladium-carbon catalyst and 1 g of borax were added to an autoclave, followed by 150 g of methylcyclohexane and 100 g of p-hydroxyanisole. The reaction was slowly heated to 100 °C and hydrogen was introduced into the system until the pressure reached 1.0 MPa, and stirring was started. When the pressure dropped to 0.5 MPa, hydrogen was supplemented to 1.0 MPa, keeping the reaction pressure in the range of 0.7-1.0 MPa. Continuously monitor the hydrogen consumption, and after the hydrogen consumption stops for a period of time, take samples for reaction process monitoring. When the remaining amount of raw material is less than 1%, the reaction is judged to be complete. The reaction mixture was cooled to 30°C and filtered to remove the catalyst. The filtrate was evaporated to remove the solvent and subsequently distilled under reduced pressure to give 92 g of p-methoxycyclohexanone in 90% yield.

150-76-5 Synthesis

150-76-5
821 suppliers
$5.00/5 g

13482-23-0
221 suppliers
$20.00/250mg

Yield:13482-23-0 90%

Reaction Conditions:

with sodium tetraborate decahydrate;palladium on activated charcoal;hydrogen at 100; under 3750.38 - 7500.75 Torr;Autoclave;

Steps:

6 Example 6
Palladium carbon 7g and borax 1g were added to an autoclave, methylcyclohexane 150g and p-hydroxyanisole 100g were added, slowly heated to 100C, hydrogen was passed to 1.0Mpa, stirring was started, and when it was reduced to 0.5Mpa ,Supply hydrogen to 1.0Mpa, and keep 0.71.0Mpa. After confirming no longer consume hydrogen for a period of time, take samples and control. When the remaining material is less than 1%, the reaction is completed. Cool down to 30°C, filter off the catalyst, and the filtrate is evaporated. In addition to the solvent, the product was distilled under reduced pressure to 92 g of p-methoxycyclohexanone at a yield of 90%.

References:

Henan Zi Wei Xing Chemical Co., Ltd.;Wu Doucan;Mao Longfei;Li Wei;Lu Zhiguo;Wang Zhenggang;Lu Biao;Jia Shuhong;Yuan Zhiguo CN107827881, 2018, A Location in patent:Paragraph 0034; 0035

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18068-06-9 Synthesis