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The synthetic method of 3-methyl-d3-benzyl bromide

A synthesis method, the technology of benzyl bromide, which is applied in the field of synthesis of 3-methyl-D3-benzyl bromide, can solve the problems of low cost and incomplete exchange of hydrogen and deuterium, and achieve the effect of stable deuterium rate

Active Publication Date: 2020-03-27
南京昊绿生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The present invention solves the problem of incomplete exchange of hydrogen and deuterium by using deuteroiodomethane as a raw material to synthesize the final product, and at the same time can achieve low cost and controllable

Method used

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  • The synthetic method of 3-methyl-d3-benzyl bromide
  • The synthetic method of 3-methyl-d3-benzyl bromide
  • The synthetic method of 3-methyl-d3-benzyl bromide

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Embodiment 1

[0036] Embodiment 1 synthetic 3-methyl-D3-benzyl bromide

[0037] In the present embodiment, the synthetic experimental method process is as follows:

[0038] step one:

[0039] The reaction scheme is as follows:

[0040]

[0041] In the low-temperature reaction tank, under the protection of nitrogen, add 20.31 g of the compound 1,3-dibromobenzene (86.1 mmol) into a three-necked bottle, add 60 ml of anhydrous tetrahydrofuran, and cool the liquid nitrogen to an internal temperature below -78°C, and keep it for 20 minutes. , slowly add 68.8 milliliters of 2.5M n-butyllithium solution (172mmol) dropwise, keep the internal temperature below -78°C, during which a large amount of solids are precipitated, after the addition is completed, after the temperature is kept at -78°C for 30 minutes, add 10.7ml of deuterium dropwise Mixed solution of iodomethane (172mmol) and 20ml of anhydrous tetrahydrofuran, the temperature was raised violently, after the slow dropwise addition was com...

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Abstract

The invention provides a synthetic method of 3-methyl-D3-benzyl bromine. The method comprises the following steps: 1) 1,3-dibromobenzene and Iodomethane-d3, which are used as raw materials, are subjected to a substitution reaction in the presence of a n-butyllithium solution, so as to prepare a compound I; 2) the compound I prepared in the step 1) and DMF(N,N-dimethyl formamide), which are used as raw materials, are subjected to a substitution reaction in the presence of a n-butyllithium solution, so as to prepare a compound II; 3) the compound II prepared in the step 2) and (NaBH4) sodium borohydride, which are used as raw materials, are subjected to a reduction reaction, so as to prepare a compound III; and 4) the compound III prepared in the step 3) and phosphorus tribromide, which are used as raw materials, are subjected to a reaction to prepare a compound IV, namely the product 3-methyl-D3-benzyl bromine. By using the Iodomethane-d3 sold in the market as the raw material for synthesis of the target product, deuterated ratio is stable and reaches a relatively high standard (D is greater than 99%).

Description

technical field [0001] The invention relates to a synthesis method of 3-methyl-D3-benzyl bromide, which belongs to the technical field of chemical synthesis. Background technique [0002] 3-Methylbenzyl bromide is a very commonly used chemical, generally used as an intermediate. [0003] The structural formula of stable isotope-labeled 3-methylbenzyl bromide, i.e. 3-methyl-D3-benzyl bromide, is as follows: [0004] [0005] 3-Methyl-D3-benzyl bromide is mainly used for pharmaceutical intermediates, to synthesize stable isotope-labeled pharmaceutical active molecules, and to provide labeling blocks for new drug research and development; it can also be used for intermediates in the direction of materials to synthesize new materials. [0006] The synthetic method of the stable isotope-labeled 3-methyl-D3-benzyl bromide of existing reports adopts the following synthetic route: [0007] [0008] The existing synthetic route has the following technical problems; [0009] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/16C07C22/04C07C17/269C07C25/02C07C29/14C07C33/20C07C45/00C07C47/542
CPCC07B2200/05C07C17/16C07C17/269C07C29/14C07C45/004C07C22/04C07C25/02C07C33/20C07C47/542
Inventor 贲昊玺
Owner 南京昊绿生物科技有限公司
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