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Catalysts 2020, 10, 762 8 of 15 Catalysts 2020, 10, x FOR PEER REVIEW 8 of 16 butitwas60st°iClloart1a6n0–a1c8c0ebpatraobfleClOe2vaetl.40N°eCv,e8rtmhLe/lmesins,4h5igmhinv)aclounedsitiofnsc.TTOheNpwrodeurectoybietladisnwedere(941–956), determined by GC-MS. The extraction yields refer to the mass of products and reactants. showing good system activity. To investigate the possible cause of the gradual decrease in catalyst activity during the subsequent To investigate the possible cause of the gradual decrease in catalyst activity during the runs, extracts after the first, second, fifth and eighth runs were analyzed by inductively coupled subsequent runs, extracts after the first, second, fifth and eighth runs were analyzed by inductively plasma–mass spectrometry (ICP-MS). The highest ruthenium content was observed for extracts after coupled plasma–mass spectrometry (ICP-MS). The highest ruthenium content was observed for the first and second runs (7.1–6.6 ppm) if n-heptane was applied regardless of the IL used. A pale extracts after the first and second runs (7.1–6.6 ppm) if n-heptane was applied regardless of the IL yellow color was visible in both extracts. Although extracts analyzed after the fifth and eighth cycles used. A pale yellow color was visible in both extracts. Although extracts analyzed after the fifth and wereecioglhotrhlecsysc,letshwereurethcoelnoirulemss,ctohnetreuntthewnaiusmoncloyntaenbtitwlaoswoenrly(6a.4b–it4l.o8wpeprm(6.)4.–C4.l8eparplmy)b.eCtltearrlryesbuetltesrwere obserrveesudltwswhenresocbCseOrvewdawshuensesdcCaOs2awnaesxutsreadctasnatn.eFxotraactlalnItL.sF,oruatlhlIeLnsi,urmuthceonniutemntcointetnhteinanthaelyzed 2 analyzed extracts was comparable and lower than < 1 ppm. It should be pointed out that, despite extracts was comparable and lower than < 1 ppm. It should be pointed out that, despite significantly significantly lower catalyst leaching in scCO2, the activity of catalytic systems was the same as for lower catalyst leaching in scCO2, the activity of catalytic systems was the same as for processes processes that used n-heptane for extraction. Thus, a gradual decrease in catalyst activity is rather that used n-heptane for extraction. Thus, a gradual decrease in catalyst activity is rather caused caused by the formation of inactive catalyst species or non-coordinative cyclohexylphosphine oxide by the formation of inactive catalyst species or non-coordinative cyclohexylphosphine oxide than than catalyst leaching. Similar observations were made by us during recyclable hydroboration of catalyst leaching. Similar observations were made by us during recyclable hydroboration of alkynes in alkynes in [Ru(CO)Cl(H)(PPh3)3]@[EMPyr][NTf2] or [Ru(CO)Cl(H)(PPh3)3]@[EMPyr][OTf]/scCO2 [Ru(CO)Cl(H)(PPh ) ]@[EMPyr][NTf ] or [Ru(CO)Cl(H)(PPh ) ]@[EMPyr][OTf]/scCO systems [30]. systems[30]. 33 2 33 2 2.4. Repetitive Batch Borylative Coupling in the Biphasic Solvent System—[Ru(CO)Cl(H)(PCy ) ]@ILs/scCO 2.4. Repetitive Batch Borylative Coupling in the Biphasic Solvent System— 3 2 2 [Ru(CO)Cl(H)(PCy3)2]@ILs/scCO2 In the final stage of our study we performed a repetitive borylative coupling of 1 with 2a, 2d and 2j inItnhtehebfiipnhalastiacgecaotfaoluyrtisctusdyystweme pe[Rrfuor(mCOed)Ca rl(eHpe)t(iPtiCveyb)or]y@la[tBivMe cImou]p[OlinTgf]o/fs1cCwOith 2(aF,ig2duraend3a–c), 2j in the biphasic catalytic system [Ru(CO)Cl(H)(PCy3)2]@[BMIm][OTf]/scCO2 (Figure 3a–c), respectively). The reactions were performed in 10-mL autoclaves equipped with sapphire windows respectively). The reactions were performed in 10-mL autoclaves equipped with sapphire windows under optimized reaction and extraction conditions at 180–190 bar of scCO2 (Figure 3d). Similar to the under optimized reaction and extraction conditions at 180–190 bar of scCO2 (Figure 3d). Similar to repetitive trans-borylation of 1 with 2a in [Ru(CO)Cl(H)(PCy3)2]@[BMIm][OTf], very high reaction the repetitive trans-borylation of 1 with 2a in [Ru(CO)Cl(H)(PCy3)2]@[BMIm][OTf], very high reaction and extraction yields of 3a in the biphasic solvent system, were observed. Cumulative TON values and extraction yields of 3a in the biphasic solvent system, were observed. Cumulative TON values were comparable to those obtained for the monophasic system (930 vs. 924). were comparable to those obtained for the monophasic system (930 vs. 924). 322 Figure 3. Repetitive batch borylative coupling of 1 with 2a (a), 2d (b) and 2j (c) in Figure 3. Repetitive batch borylative coupling of 1 with 2a (a), 2d (b) and 2j (c) in [Ru(CO)Cl(H)(PCy ) ]@[BMIm][OTf]/scCO biphasic solvent systems under optimized reaction [Ru(CO)Cl(H)(P3C2y3)2]@[BMIm][OTf]/scCO22biphasic solvent systems under optimized reaction ([Ru- ◦ ([Ru-H]:1::2aa,,22ddoorr2j2j==0.01.0:11:1:1.5:,1.151,01°1C0, 6Ch,,61hg,o1fg[BoMfIm[B]M[OITmf]],[OineTrft],atimneorstphatemreocsopnhdeitrieoncso)nadnidtions) and extraction (160–180 bar of CO2 at 40 ◦C, 8 mL/min, 45 min) conditions. Visualization of the reaction mixture through the sapphire window of high-pressure autoclave’s (d). The product yields were determined by GC-MS. The extraction yields refer to the mass of products and reactants.PDF Image | Ru-Catalyzed Repetitive Batch Borylative Coupling of Olefins
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