Preparation method of 3-oxetane potassium trifluoroborate_Industrial additives

Formylbenzeneboronic acid

Background and overview of the preparation method of 3-oxetane potassium trifluoroborate

3-oxetane potassium trifluoroborate can be used as a pharmaceutical synthesis intermediate. If 3-oxetane potassium trifluoroborate is inhaled, move the patient to fresh air; if skin contact occurs, remove contaminated clothing, rinse the skin thoroughly with soap and water, and seek medical attention if you feel unwell; If eye contact occurs, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.

Preparation method of 3-oxetane potassium trifluoroborate

Preparation of 3-oxetane potassium trifluoroborate is as follows: Weigh B2pin2 (1.5 equiv), LiOMe (2.0 equiv), PS-PPh3 (13 mol%) and CuI (10mol%). The flask was closed with a septum, evacuated, and backfilled with N2. DMF (5 mL) and halide (1.0 mmol, 1.0 equiv) were added sequentially via syringe (or, if the halide was a solid, added as a solution in DMF), and the reaction was stirred vigorously at room temperature for 20 h. The reaction mixture was then diluted with CH2Cl2 (10 mL), filtered through a pad of celite, and rinsed with CH2Cl2 (20 mL). The resulting solution was concentrated and poured into a saturated solution. Extract three times with aqueous NH4Cl solution (20 mL) and Et2O (20 mL). The combined organic layers were washed with H2O (50 mL) and brine (50 mL), dried (MgSO4) and concentrated. Dissolve the residue in THF (5 mL) in a round-bottomed flask equipped with a stir bar and let stand. Add aqKHF2 (4.5M, 0.9mL, 4.0eq). The flask was closed with a septum and the resulting mixture was stirred at room temperature for 2 hours. The reaction mixture was evaporated to dryness and the resulting salt was extracted several times with hot acetone. The filtrate was concentrated to approximately 5 mL and precipitation was achieved by adding dropwise the filtrate into Et2O (100 mL) at 0 °C. The resulting product was collected by gravity filtration on a sintered funnel and dried to give the corresponding 3-oxetane potassium trifluoroborate as a white solid.