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An important synthesis process of fluorine intermediate

A kind of synthesis technique, the technology of intermediate

Active Publication Date: 2020-09-15
BIRDO (SHANGHAI) PHARMATECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] A preparation method of the compound is disclosed in the WO patent application with the publication number WO2017020065A1 (another Journal of Medicinal Chemistry, 2013, vol.56, #3p.640-659), the preparation method is as follows Reaction formula (Route 1) Carrying out: However, the reaction process is easy to convert incompletely, causing the raw materials and products to be difficult to separate, and the reaction yield is very low, only 30%

Method used

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  • An important synthesis process of fluorine intermediate
  • An important synthesis process of fluorine intermediate
  • An important synthesis process of fluorine intermediate

Examples

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Effect test

Embodiment 1

[0028] Example 1: An important synthetic process for fluorine intermediates, prepared through the following steps:

[0029] (1) Add 400g compound 1 and 2.5L methanol in the reaction flask, cool down in an ice bath, stir, and slowly add dropwise a solution composed of 200g trifluoroacetic acid and an organic solvent for 40min. The organic solvent is methanol. After the dropwise addition, at 25 Stirred under the condition of ℃ for 6 hours, spin-dried to obtain 557g of compound A shown in chemical formula A, the yield was 99%, LCMS (M+H): 226.1;

[0030] (2) Add 550g of Compound A and 3.0L of organic solvent in sequence in the reactor. The organic solvent is methanol. Add 314g of fluorine reagent in batches under ice bath. The fluorine reagent is 1-chloromethyl-4-fluoro-1,4- Diazotization of bicyclic 2.2.2-octane bis(tetrafluoroborate), naturally warming up to 20°C, stirring for 1 hour, monitoring the reaction by TLC until the raw materials disappeared, adding ammonia methanol so...

Embodiment 2

[0032] Example 2: An important synthetic process for fluorine intermediates, the difference from Example 1 is that R1 and R2 are both ethyl groups.

Embodiment 3

[0033] Example 3: An important synthetic process for fluorine intermediates, the difference from Example 1 is that R1 and R2 are both propyl groups.

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Abstract

The invention discloses an important fluorine intermediate synthesis process, and relates to the technical field of chemical synthesis. According to the present invention, the synthetic process is environmentally friendly, and by synthesizing the intermediate for forming the salt, the stability of the intermediate compound is easily achieved, the solubility of the intermediate as the reactant in the next step is easily achieved, the yield of the product can achieve 66-75%, the purity can achieve 95-98%, the product yield is significantly improved, and the high economic benefits can be obtained; and the synthesis process has characteristics of easy operation, easily-controlled process conditions and cost reducing, and is suitable for mass production.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, more specifically, it relates to an important synthesis process of fluorine intermediates. Background technique [0002] CDK4, CDK6 / cyclinD will produce severe symptoms such as lung cancer, breast cancer, brain cancer and central nervous system diseases, colorectal cancer and leukemia when they are overexpressed. Scientists have discovered a new class of very effective enzyme inhibitors, The compound represented by the following chemical formula 1 is a common effective structure, and the most commonly used intermediate for synthesizing this type of compound is the fluorine intermediate shown in chemical formula 2. [0003] [0004] A preparation method of the compound is disclosed in the WO patent application with the publication number WO2017020065A1 (another Journal of Medicinal Chemistry, 2013, vol.56, #3p.640-659), the preparation method is as follows Reaction formula (Route 1) ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/42C07B39/00
Inventor 王雷王晓磊陈达
Owner BIRDO (SHANGHAI) PHARMATECH CO LTD
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