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US 7,910,078B2 78 removed and the solutionWas stirredatroom temperature for 3h.ItWasdilutedWith30mL ofmethanolandthencooledin ice Water. Sodium boron hydride (26 g, 0.68 mol) Was added slowly. Cooling Was removed after the addition Was com pletedin1h.The stirringWas continuedatroomtemperature for3h,atWhichtime30mL ofsaturatedsodiumchlorideWas addedandthemixtureWas stirredforadditional1h.Thecolor of the solution turned from green dark into Wine red. The formed solid Was ?ltered off through Buchuel funnel, and WashedWithdichloromethane.TheorganiclayerWassepa 10 rated and the aqueous layer Was extracted With dichlo romethane (><3). The combined organic layers Were dried (Na2SO4), ?ltered and concentrated under reduced pressure. A totaloffourbatchesofbenchreactionproductsWerecom bined and fractionally distilled using a viqreux column to afford 4-(diethylamino)-2-butanol (260 g, 66%): bp 110° C./50-55mmHg; IR(neat)3383(br.),2966,1465cm_l;1H NMR (CDCI3,500MHZ) 53.89(tq,J:2.1,6.2HZ,1H), 2.58-2.69 (m, 3H), 2.52 (dt, 1:38, 13.0 HZ, 1H), 2.31 (sex, J:7.1HZ,2H),1.48-1.58(m,1H),1.39(dq,1:35,14.4HZ,20 1H), 1.10 (d, 1:62 HZ, 3H), 1.00 (t,J:7.2 HZ, 6H). 3H, 1:62 HZ), 1.20-1.56 (m, 2H), 2.41-2.94 (m, 3H), 3.75 3.92(m,1H)(NHandOH notobserved). Example2 Synthesis of the amino alcohol 4-(morpholino)-2-butanol(2)4Comparative Example Me 2)NaBH4 0y 25 30 35 ExpansionoftheprotocolinExample 1to4-(piperidino) 2-butanol(4)Wasaccomplishedbysimplychangingthe diethyl amine to piperidine. IR vmax: 3075-3600 cm_l; 1H NMR, 6(200MHZ,CDCl3):1.16(d,3H,1:8HZ),1.35-1.70 (m,8H),2.15-2.38(m,2H),2.45-2.60(m,4H),3.85-4.00(m, 1H). Example 5 Synthesis of the amino alcohol 1-dimethylamino-2-methyl-3-pentanol(5) ComparativeExample ExpansionoftheprotocolinExample1to4-(morpholino) 40 2-butanol (2) Was accomplished by simply changing the diethyl amine to morpholine. IR vmax: 3075-3600 cm_l; 1H NMR, 6(200MHZ,CDCl3):0.90(d,3H,1:6HZ),1.15-1.50 (m,2H),2.05-2.45(m,6H),3.42(t,4H,1:46HZ),3.60-3.78 (m,1H),5.22-5.36(brs,1H). A solutionof3-pentanone(87g,1.0mol),dimethylamine hydrochloride (93.8 g, 1.15 mol), parafonnaldehyde (33 g, 1.10 mol) and concentrated hydrochloride acid (1 mL) in anhydrousethanol(90mL)Washeatedatre?uxfor1day.The solvent Was removed under reduced pressure. The remaining material Was cooled in an ice Water bath and treated With an aqueous solution of 40% sodium hydroxide (50 mL), fol loWed by solid sodium hydroxide (30 g). The mixture Was stirredfor30minutes.Subsequently,itWas?lteredthrougha short pad of CeliteTM and Washed With diethyl ether. The mixture Was then thoroughly extracted With diethyl ether (x2), and the organic layers Were dried With Na2SO4, ?ltered andevaporated.TheremainingmaterialWaspuri?edbyfrac tionaldistillationundervacuumtogivetheaminoketone (102.8 g, 72%) as a colorless oil: bp 1050 C./52 mmHg; IR (neat)2966,2942,2766,1707,1454cm_l;1HNMR (CDCI3, 500 MHZ) 6 2.70-2.80 (m, 1H), 2.54-2.62 (m, 1H), 2.44-2.54 (m,2H),2.18(s,3H),2.19(s,3H),2.10-2.16(m,1H),0.80 1.80(m,6H);13CNMR(CDCI3,125MHZ)6214.2(C),62.8 (CH2), 45.6 (CH3), 44.2 (CH), 34.4 (CH2), 15.0 (CH3), 7.3 (CH3) Subsequently,theketone(90g,0.63mol)WasdilutedWith methanol(30mL) andcooledinaniceWaterbath.Thesolu tionWassloWlytreatedWithNaBH4(29g,0.76mol)overa period of 1 hour. After stirring continuously at 0° C. for Example3 Synthesis of the amino alcohol 4-(isopropylamino)-2-butanol(3) 45 50 55 60 ExpansionoftheprotocolinExample 1to4-(isopropy lamino)-2-butanol(3)Wasaccomplishedbysimplychanging65 the diethyl amine to isopropylamine. IR vmax: 3075-3600 cm_l;1HNMR,6(200MHZ,CDCl3):0.85(d,6H),1.04(d, another1hourandatroomtemperaturefor3hours,the Example4 Synthesis of the amino alcohol 4-(piperidino)-2-butanol(4) OHPDF Image | METHOD OF CAPTURING CARBON DIOXIDE FROM GAS STREAMS
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