2-(2-甲氧基乙氧基)苯基硼酸

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 500 mg pulverized molecular sieves (4 Å), the compound of step 2 (761 mg, 3.88 mmol), 2-chloro-1H-indole-3-carbaldehyde (465 mg, 2.59 mmol) and copper(II) acetate (940 mg, 5.18 mmol) in DCM (20 ml) was added pyridine (0.42 ml, 5.18 mmol) and triethylamine (0.72 ml, 5.18 mmol). The reaction mixture was stirred at room temperature for one week. The mixture was diluted with water and extracted with DCM. The organic layer was separated, dried over sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by preparative HPLC. The eluate was lyophilized overnight to give 56 mg of the title compound. To a suspension of 500 mg extracted with DCM The organic layer was separated dried over sodium sulfate filtered evaporated under reduced pressure The residue was purified by preparative HPLC

反应条件: temp:-78.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of the compound of step 1 (2.20 g, 7.91 mmol) in toluene (20 ml) and THF (4 ml) was added triisopropyl borate (2.19 ml, 9.49 mmol), and the mixture was cooled to −78° C. n-Butyllithium (3.79 ml, 9.49 mmol, 2.5 M in hexane) was added dropwise and the reaction mixture was stirred at −78° C. for 1.5 h. The cooling bath was removed and the reaction mixture was allowed to warm to −20° C. Then 2 N hydrochloric acid (7 ml) was added. When the mixture had reached room temperature, water and EA were added. The organic layer was separated, dried over sodium sulfate, filtered and evaporated in vacuo. The residue was purified by silica gel chromatography (EA/HEP 1:4). 766 mg of the title compound were obtained. was added dropwise The cooling bath was removed to warm to −20° C Then 2 N hydrochloric acid (7 ml) was added had reached room temperature water and EA were added The organic layer was separated dried over sodium sulfate filtered evaporated in vacuo The residue was purified by silica gel chromatography (EA/HEP 1:4)