Application background and overview of boron trifluoride tetrahydrofuran complex in the synthesis of 3-mercapto-1-propanol
Boron trifluoride tetrahydrofuran complex, also called boron trifluoride tetrahydrofuran, is a chemical with the molecular formula C4H8BF3O. It is mainly used as a catalyst for organic reactions, chemical reagents and pharmaceutical intermediates.
Application of boron trifluoride tetrahydrofuran complex in the synthesis of 3-mercapto-1-propanol [1]
Boron trifluoride tetrahydrofuran complex is used to synthesize 3-mercapto-1-propanol. 3-Mercapto-1-propanol is an important intermediate for the preparation of medicines, pesticides, and electronic materials. In industry, 3-mercapto-1-propanol is an important fine chemical raw material. Therefore, 3-mercapto-1-propanol has good market prospects.
CN20161110064 Boric acid-10B8.1 provides a preparation method of 3-mercapto-1-propanol with low cost, high purity, simple operation and controllable quality. In order to achieve the above object, the technical solution adopted by the present invention is a preparation method of 3-mercapto-1-propanol, which includes the following steps: adding tetrahydrofuran and 3-mercaptopropionic acid into the reaction kettle, and then adding tetrahydrofuran and 3-mercaptopropionic acid into the reaction kettle, and then adding ℃, add sodium borohydride in batches and stir continuously. After the sodium borohydride is added dropwise, stir for 30 minutes, then slowly add boron trifluoride tetrahydrofuran complex solution dropwise at this temperature, raise the temperature to 30~40°C and keep it for 4 ~6 hours, then raise the temperature to 50~60°C and keep it for 1~1.5 hours to obtain a solid mixture, which is then cooled to room temperature. Slowly add water dropwise, then evaporate the tetrahydrofuran. After cooling to room temperature, add 33%wt hydrochloric acid to adjust the pH to 2~3, then add chloroform, filter, separate and distill to collect 3-mercapto-1-propanol. The optimal molar ratio of 3-mercaptopropionic acid and sodium borohydride is 1:1.5~1.7. The optimal molar ratio of mica in the 3-mercaptopropionic acid and boron trifluoride tetrahydrofuran complex is 1:0.8~1.0.
The reaction formula of the preparation method of 3-mercapto-1-propanol of the present invention is as follows:
The beneficial effects produced by the present invention are: the raw materials used in the preparation of 3-mercapto-1-propanol are all commonly used chemicals, the price of raw materials is low, and the cost is saved; sodium borohydride is used to complex with boron trifluoride and tetrahydrofuran Borane is obtained from the reaction of the substance, and 3-mercaptopropionic acid is directly reduced. The conditions are mild and simple, which improves the safety during the operation; and the yield of 3-mercapto-1-propanol can reach more than 80%, and the product purity can be Reaching more than 99.3%; the preparation process has little pollution, the organic solvents tetrahydrofuran and chloroform used can be recycled, and the boric acid produced by post-processing can be recycled through concentration and recrystallization, making it suitable for industrial production.
