苄基(二氯)硼烷

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

实验步骤: About 10.0 ml (11.51 grams, 66.6 mmoles) of benzyl dichloroborane is dissolved in 100 ml of toluene in a 500 ml three-neck flask. Research grade acetylene is passed at a rate of 100 ml STP/min through two dry ice/acetone traps and a column (10 inches long ×1 inch ID) of activated basic alumina. The acetylene is introduced into the stirring solution through a needle below the surface of the liquid. The flask is vented to a scrubber containing 2.7 grams of NaOH in 1500 ml of water. The reaction is allowed to proceed for 3 hours. The acetylene flow is stopped and the volatiles in the reaction flask are evaporated under vacuum. 10.37 grams of colorless product are recovered. This is identified as 2-chloro-1,2-dihydro-2-boranaphthalene by NMR. This product is used in subsequent steps without further purification. The yield is 95 %. the volatiles in the reaction flask are evaporated under vacuum 10.37 grams of colorless product are recovered This product is used in subsequent steps without further purification