71597-85-8Relevant articles and documents
Method for preparing boric acid derivative (by machine translation)
-
Paragraph 0038-0039; 0046-047, (2020/12/29)
The invention provides a preparation method of p-hydroxyphenylboronic acid. The method is characterized by comprising the following -0.1 mpa steps: at 0 - 10 °C vacuum conditions and temperature, heating the alkoxyl phenylboronic acid and acid first chloride compound in organic solvent, then heating the aqueous layer minutes every interval until 10 °C 15 the temperature is raised to, and then 30 - 100 °C carrying out 1 - 2h constant temperature reaction to obtain the intermediate pH. The aqueous layer 9-11 is further recrystallized by organic solvent 3-4 to obtain intermediate compound and second alkali adjusting system pH. 3rd. The p-hydroxyphenylboronic acid is obtained. The method has the advantages that the reaction temperature is relatively mild, the reaction time can be obviously shortened, the consumption of the catalyst is reduced, and the method has higher yield and purity. (by machine translation)
Preparation method of hydroxyphenylboronic acid
-
, (2020/05/08)
The invention discloses a preparation method of hydroxyphenylboronic acid, which belongs to the technical field of boric acid synthesis in medical intermediates. The method comprises the following steps: starting from bromophenol, carrying out BOC, trimethylsilyl or benzyl protection, forming a Grignard reagent, reacting with borate, or carrying out one-pot reaction with borate and n-butyllithium,and hydrolyzing to obtain hydroxyphenylboronic acid. According to the invention, cheap and easily available protecting groups are adopted, so that the protecting groups are easy to remove during boronation reaction hydrolysis, industrial amplification is easy to realize, batch production is carried out on the scale of dozens of kilograms, and the process stability is good.
Bedford-type palladacycle-catalyzed miyaura borylation of aryl halides with tetrahydroxydiboron in water
Zernickel, Anna,Du, Weiyuan,Ghorpade, Seema A.,Sawant, Dinesh N.,Makki, Arwa A.,Sekar, Nagaiyan,Eppinger, J?rg
, p. 1842 - 1851 (2018/02/23)
A mild aqueous protocol for palladium catalyzed Miyaura borylation of aryl iodides, aryl bromides and aryl chlorides with tetrahydroxydiboron (BBA) as a borylating agent is developed. The developed methodology requires low catalyst loading of Bedford-type palladacycle catalyst (0.05 mol %) and works best under mild reaction conditions at 40 °C in short time of 6 h in water. In addition, our studies show that for Miyaura borylation using BBA in aqueous condition, maintaining a neutral reaction pH is very important for reproducibility and higher yields of corresponding borylated products. Moreover, our protocol is applicable for a broad range of aryl halides, corresponding borylated products are obtained in excellent yields up to 93% with 29 examples demonstrating its broad utility and functional group tolerance.