- Preparation method of 4-chloromethyl benzoyl chloride
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The invention discloses a preparation method of 4-chloromethyl benzoyl chloride, wherein the preparation method comprises the steps: (1) a step of undergoing a chlorination reaction of 4-methylebnzenemethanol with chlorine gas under the action of a catalyst dibenzoyl peroxide to prepare a 4-hydroxymethyl trichlorobenzene crude product; (2) a step of undergoing a hydrolysis reaction of the 4-hydroxymethyl trichlorobenzene crude product prepared in the step (1) with water; and (3) a step of undergoing an acylation reaction of the hydrolysis product of the step (2) with excessive oxaloyl chlorideunder the action of a catalyst DMF, to prepare the target product 4-chloromethyl benzoyl chloride. The process has the advantages of easy availability of raw materials, low price, simple operation, fewer side reactions in the whole process, low energy consumption, high product quality, low product cost, and fewer three wastes; the total product yield is 85-90% and the purity is 99% or more.
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Paragraph 0019; 0027; 0029; 0031; 0033; 0035; 0037
(2018/10/26)
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- C-F bond cleavage enabled redox-neutral [4+1] annulation via C-H bond activation
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Using α,α-difluoromethylene alkyne as a nontraditional one-carbon reaction partner, a synthetically novel method for the construction of isoindolin-1-one derivatives via Rh(III)-catalyzed [4+1] annulation reaction is reported. The 2-fold C-F bond cleavage not only enables the generation of desired product under an overall oxidant-free condition but also results in a net migration of carbon-carbon triple bond. In addition, the present reaction protocol exhibits a tolerance of a wide spectrum of functional groups due to the mild reaction conditions employed.
- Wang, Cheng-Qiang,Ye, Lu,Feng, Chao,Loh, Teck-Peng
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supporting information
p. 1762 - 1765
(2017/02/15)
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