28940-11-6Relevant articles and documents
KI-catalysed synthesis of 4-methylcatechol dimethylacetate and fragrant compound Calone 1951
Zhang, Ya-Zheng,Yang, Qian,Huang, Shao-Jian,Luo, Zi-Ping,Li, Wen-Ping,Dong, Li-Chun
, p. 586 - 593 (2013)
Synthesis of the fragrant compound Calone 1951 from 4-methyl catechol and methyl bromoacetate entails three successive reactions: the Williamson reaction, Dieckmann condensation, and hydrolysis-decarboxylation reaction. In this paper, the synthesis of 4-methylcatechol dimethylacetate (MCDA) via the Williamson reaction by adding KI as catalyst was investigated. It was found that the addition of an appropriate amount of KI can significantly increase the product yield due to generation of methyl iodoacetate via the reaction between KI and methyl bromoacetate. The synthesised MCDA as well as Calone 1951 were first characterised by melting points, HPLC, IR, and NMR analyses. Next, the effect of the key operating factors on MCDA synthesis by the Williamson reaction was investigated and the optimum operating conditions were obtained via a group of orthogonal experiments. The verification experiments demonstrated that, under the optimum operating conditions, the MCDA yield could be increased from 78.5 % to 95.4 % by the addition of an appropriate amount of KI; the corresponding yield of Calone 1951 increased to 68 %.
Method for synthesizing watermelon ketone
-
Paragraph 0034-0059, (2021/11/19)
The invention belongs to the technical field of perfume compound synthesis. The invention specifically relates to a synthesis method of watermelon ketone. The method comprises the following steps: adding a solvent and a periodate into the reaction vessel at room temperature, stirring uniformly, and then dropwise adding the watermelon ketone precursor alcohol (I) dissolved by the solvent to the reaction vessel to obtain a crude watermelon ketone crude product which is subjected to recrystallization to obtain the watermelon ketone (3 - 7h II) finished product. To the invention, 4 - methylcatechol and 1, 3 -dichloropropanol reaction product 3, 4 - dihydro -7 - methyl - 2H - 1 and 5 - benzoxazole -3 - alcohol (I) are used as starting materials and are subjected to high-iodine reagent oxidation reaction. High yields were obtained. The high-purity citrulline (II) has the advantages of simple process, high product yield, high purity and low cost, and is suitable for industrial production.
A Deoximation Method for Deprotection of Ketones and Aldhydes Using a Graphene-Oxide-Based Co-catalysts System
Tong, Qiaolin,Liu, Yang,Gao, Xuezhi,Fan, Zhanfang,Liu, Tianfu,Li, Bo,Su, Dangsheng,Wang, Qinghe,Cheng, Maosheng
supporting information, p. 3137 - 3145 (2019/05/01)
The deoximation of a wide range of ketoximes and aldoximes to their corresponding carbonyl compounds with high yields has been achieved using graphene oxide (GO) and sodium nitrite (NaNO2) as highly efficient catalysts and air as the green oxidant under mild conditions. The mechanism of deprotection and recycling use of catalyst were revealed in deep experiment. The carboxylic acid groups on the GO were essential for high catalytic activity. (Figure presented.).