TETRAKIS(PYRROLIDINO)DIBORANE 95 synthesis

Yield:158752-98-8 71%

Reaction Conditions:

with sodium in toluene at 105 - 110;Inert atmosphere;

Steps:

1 Example 1

Under nitrogen protection,Sodium metal (2.6 g, 0.11 mol) and 20 mL of toluene,After heating to 100 ° C until the metal sodium is completely dissolved,Start rapid stirring and continue to raise the temperature to 105-110 °C.Bis(tetrahydropyrrole) boron bromide (21.8 g, 0.094 mol) was dissolved in 6 mL of toluene.Start to add dropwise to the above metal sodium toluene solution, and maintain a weak reflux state during the dropwise addition.After the addition is completed, the mixture is stirred for 3-5 hours, and the system is dark blue.The sample was detected by GC and the internal standard yield of the reaction solution was 79%.At this time, a solution of chlorocyclopentane (0.4 mol) / toluene (15 mL) was added dropwise, and the addition was completed.The reaction was stirred for 2 hours. At this time, the internal standard yield of the reaction liquid was 78%, filtered, and the solid was washed with toluene, and the filtrate was distilled under reduced pressure. After the low-boiling impurities were distilled, n-heptane was added.55mL, gradually cooled to below -20 °C with stirring.Filtration gave 10.1 g of a light yellow solid coupled product in a yield of 71%.

References:

CN109608484,2019,A Location in patent:Paragraph 0017