52589-39-6Relevant articles and documents
Measurement of the Dissociation of EuII-Containing Cryptates Using Murexide
Lenora, Chamika U.,Staples, Richard J.,Allen, Matthew J.
, p. 86 - 93 (2020)
The dissociation rates of five EuII-containing cryptates in water were measured using UV-visible spectroscopy and murexide at pH 6.5, 7, 7.5, 8, and 9. Murexide was used as a coordinating dye for EuII. The results for a known cryptate were within experimental error of the value obtained using other methods and enabled the measurement of other cryptates. This validation of the use of murexide to study the dissociation of EuII-containing cryptates enables its use with other complexes of EuII
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 (2013/07/26)
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 %.
Microwave assisted synthesis of the fragrant compound Calone 1951
Drevermann, Britta,Lingham, Anthony,Hügel, Helmut,Marriott, Philip
, p. 39 - 41 (2007/10/03)
Microwave irradiation has been utilised in a three-step synthetic route to the fragrant compound, 7-methyl-benzo[b][1,4]dioxepin-3-one, commercially known as Calone 1951. The use of a microwave reactor increases the simplicity and efficiency of the overall synthesis. Calone 1951, 7-methyl-benzo[b][1,4]dioxepin-3-one, possesses a strong marine, ozone note with floral nuances and is synthesised via a three-step procedure using microwave irradiation. High yields were obtained, and reaction times reduced to a few minutes, allowing for an efficient and inexpensive synthesis of Calone 1951.