反应详情

温度

90 °C

To a 20 L four-neck bottle tri-isopropyl borate (261.0 g, 1.388 mol) and pinacol (142.5 g, 1.207 mol) were added and heated to ˜90° C. for 12-16 h. The criteria for a reaction completion is pinacol<4.0% by GC. After completion, the reaction was converted to distillation, and the product fractions (boiling at 174-178° C.) collected. Thus the title product was obtained as a colourless oil in a yield range of 80-90% th across the six 20 L batches which were operated. GC records purity of 87-96%, but 1H NMR shows the product to be very pure. [discrepancy due to product instability to GC conditions.]

1. distillationAfter completion, the reaction was converted to distillation
2. customthe product fractions (boiling at 174-178° C.) collected