Industrial production method of 9-iodo-9-borabicyclo[3.3.1]nonane solution

By controlling the ventilation time and ventilation amount of hydrogen iodide gas in a heterogeneous system and optimizing the reaction conditions, the problems of high production cost and low yield of 9-iodo-9-borazobile[3.3.1]nonane in the prior art are solved, and industrial production with high purity and high yield is achieved, which is suitable for safe production.

CN115850309BActive Publication Date: 2025-09-02SHANGHAI FULE PHARM TECH CO LTD
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Patent Information

Application Number
CN202211445401.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-11-18
Publication Date
2025-09-02
Estimated Expiration
2042-11-18

AI Technical Summary

Technical Problem

The existing synthesis method of 9-iodo-9-boranone [3.3.1]nonane has problems such as high production cost, low yield, many impurities, and unsuitable for industrial production. In particular, the homogeneous reaction system is difficult to control the equivalent ratio and the purification process is complicated.

Method used

The 9-boronabicyclic[3.3.1]nonane dimer is used to react with hydrogen iodide gas in a heterogeneous system. By controlling the ventilation time, ventilation amount and temperature of the hydrogen iodide gas, the reaction conditions are optimized to form a high-purity 9-iod-9-boronabicyclic[3.3.1]nonane solution.

Benefits of technology

The industrial production of 9-iodo-9-borazobile[3.3.1]nonane solution with low cost, high yield and high purity is achieved, which is suitable for safe production. The product can be used directly for reaction without additional purification.

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Abstract

The present invention provides an industrial production method for a 9-iodine-9-borane bicyclo[3.3.1] solution, comprising the steps of: 1) passing an appropriate amount of dry hydrogen iodide gas generated on site into a mixture of a 9-borane bicyclo[3.3.1]nonane dimer and an organic solvent under inert gas protection at 15 to 25° C. to carry out a heterogeneous system reaction; 2) after stopping the introduction of hydrogen iodide, stirring for 1 to 20 hours at 15 to 25° C., degassing the mixture by vacuum pumping negative pressure for 5 to 10 minutes and replenishing nitrogen to obtain a colorless transparent solution, which is then appropriately diluted to obtain a commercially available 9-iodine-9-borane bicyclo[3.3.1]nonane solution. The present invention is suitable for the industrial production of a 9-iodine-9-borane bicyclo[3.3.1]nonane solution and has the advantages of mild reaction conditions, safe and simple operation, low environmental production cost, and a stable production process.
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