13511-38-1Relevant articles and documents
Purification method of intermediate 4,4-dimethyl isoxazole-3-ketone
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Paragraph 0023; 0029; 0036; 0042; 0049; 0055; 0062; 0066;, (2021/01/25)
The invention discloses a purification method of an intermediate 4,4-dimethyl isoxazole-3-one, which comprises the following steps: washing a 4,4-dimethyl isoxazole-3-one reaction solution with pure water until the pH value of the oil phase of the reaction solution is 7.5-9.0, dissolving with alcohol, distilling, refluxing, acidifying, crystallizing and filtering to obtain the solid 4,4-dimethyl isoxazole-3-one with a purity of 99.5% or above. The purification process is simple, the post-treatment is highly operable, the key technical problems of low product purity, difficulty in refining andinfluence on the purity of the subsequent product clomazone in the original 4,4-dimethyl isoxazole-3-ketone preparation technology are solved, and the purification process conforms to the concept of green economic cycle.
Sulfoximine assisted Pd(II)-catalyzed bromination and chlorination of primary β-C(sp3)-H bond
Rit, Raja K.,Yadav, M. Ramu,Ghosh, Koushik,Shankar, Majji,Sahoo, Akhila K.
, p. 5258 - 5261 (2015/01/09)
S-Methyl-S-2-pyridyl-sulfoximine (MPyS) directed bromination and chlorination of the 1°-β-C(sp3)-H bond of MPyS-N-amides is realized under the influence of N-Br/Cl-phthalimides and a Pd(II)-catalyst. The sequential halogenation and acetoxylation of α-dimethyl MPyS-N-amides constructs highly functionalized α-trisubstituted aliphatic acid derivatives. The MPyS directing group is cleaved from the halogenated products and recovered. (Chemical Equation Presented).