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Cp2ZrCl2-i-BuMgBr Reagent System - the reduction of alkenes and alkynes and two dimerization of olefins

Plastic chromatography mass spectrometry and chromatography-based Hitachi i63. In addition, the product of using high pressure liquid chromatography separation. . 3 olefins reactor (three neck bottle) full Tuo for argon, and then adding Cp2ZiCI292mg (1mmo1) and THF10mL, stirring to dissolve. Add i-BuMgBr2.4-retool the THF solution (about 2mL), stirred 1h,[link widoczny dla zalogowanych], the solution color to brown. I. i added a Octene 12g (10mmo1), stirring 20h. Reaction is completed, it acidic by adding diluted hydrochloric acid. And then extracted with ethyl ether,[link widoczny dla zalogowanych], ethyl ether layer washed, dried with anhydrous sodium sulfate. Remove the solvent residue in vain before chromatographic separation, and then use the preparative chromatography separation, that was fourteen 7-8 carbon alkyl or two methyl. The formation resultant one-dodecane as internal standard, chromatographic quantification. Structures. HNMR, MS. Other olefins, methods of operation and the same. ? 4-ene reaction of Bu has been processed by a NBS Cp. ZrC1. (1mmo1) and i-BuMgBr (2.4mmo1) reagent consisting of their own system and 1-ene (10retoo1) I, 603 - 3 way by reaction at room temperature the reaction solution by adding N-bromosuccinimide (NBS) 534rag (3retoo1),[link widoczny dla zalogowanych], stirred 1h. Reaction is complete, the acidic by adding diluted hydrochloric acid, extracted with hexane, water, dried with anhydrous sodium sulfate, after Sin, and the remaining operation and 3 to the same. Other en razor also carried out the same way. 5Cp2ZrCI with the i-BuMgBrg. ~ Reaction Cp? ZrC1z (2mmo]) and i-BuMgBr (4.8,; omo1) in THF (2omL) in the reaction solution with oxygen blowing, so that the resulting isobutene into Br: CCI solution of a bromide. Australian of the completed, CCI. Washed with aqueous sodium sulfite solution to remove excess bromine. Concentrated distillation residue was separated by liquid chromatography pendulum, which was 2-methyl-I,[link widoczny dla zalogowanych], 2 - b O butane. Products identified with the former. 6 = olefins, alkynes basic operation, product analysis with the identification and 3 to the Jiu.
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