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US 7,910,078B2 reaction Was quenched by the addition of saturated sodium chloride (30 mL). The reaction mixture Was stirred for 30 minutes. Then, itWas ?ltered through a short pad of CeliteTM and Washed With diethyl ether. The ?ltrate Was dried With NaZSO4andNaCl,?lteredandevaporated.Theremaining 5 omers)63.42-3.48(m,1H),3.28-3.34(m,1H),2.56-2.74(m, material Was puri?ed by fractional distillation to give the amino alcohol 1-dimethylamino-2-methyl-3-pentanol (60 g, 66%) asacolorlessoil:bp 125° C./98mmHg; IR (neat)3408 (br),1463cm_l;1HNMR (CDCI3,500MHZ)(tWodiastere omers)63.38-3.45(m,1H),3.26-3.32(m,1H),2.49(t, 80.0(CH),77.9(CH),62.3(CH2),57.7(CH2),47.3(CH2), 1:116HZ,1H),2.42(t,J:12.1HZ,1H),2.21(s,3H),2.20(s, 47.1 (CH2), 34.5 (CH), 34.4 (CH), 28.2 (CH2), 24.9 (CH2), 3H),2.19(s,3H),2.18(s,3H),2.00-2.12(m,2H),1.60-1.70 15.1(CH3),15.0(CH3),11.6(CH3),11.5(CH3),11.3(CH3), (m,1H),1.52-1.60(m,1H),1.34-1.44(m,1H),1.22-1.34(m, 1H),1.15(dt,1:23,6.9HZ,1H),0.96(dt,J:2.1,7.3HZ,3H), 0.91(dt,J:2.1,7.3HZ,3H),0.75(dd,1:20,6.8HZ,3H),0.68 (dd, 1:19, 6.8 HZ, 3H), 0.80-0.88 (m, 1H); 13C NMR (CDCl3, 125 MHZ) (tWo diastereomers) 6 79.9 (CH), 77.1 (CH),67.8(CH2),63.3(CH2),45.7(CH3),45.3(CH3),34.4 (CH),34.0(CH),27.7(CH2),24.8(CH2),14.8(CH3),14.1 20 (CH3),10.9(CH3),8.9(CH3). 9.40(CH3). Example 6 Synthesis of the amino alcohol 1-diethylamino-2-methyl-3-pentanol (6)iComparativeExample 1.cnzo, EtZNH-HCI 2.NaBH4 25 30 Example7 Synthesis of the amino alcohol 1-dimethylamino-4,4-dimethyl-3-pentanol (7)4ComparativeExample 1.cnzo,MeZNH-HCI 2.NaBH4 OH Expansion of the protocol in Example 5 to 1-dimethy lamino-4,4-dimethyl-3-pentanol (7) Was accomplished by simplychangingthe3-pentanonetopinacolone.A suspen sionofpinacolone(50g,0.5mol),dimethylaminehydrochlo ride(46.9g,0.58mol),paraformaldehyde(16.5g,0.55mol) andaceticacid(0.5mL)inanhydrousethanol(50mL)Was heated at re?ux for 1 day. The solvent Was removed under reduced pressure during Which time the reaction mixture became solidi?ed. The solid Was cooled in an ice Water bath andtreatedWithanaqueoussolutionof30% sodiumhydrox ide(30mL),folloWedbysolidsodiumhydroxideuntilthepH Was >10. The mixture Was ?ltered through a short pad of CeliteTM and Washed With diethyl ether. The mixture Was then thoroughlyextractedWithdiethylether(x3),andtheorganic layers Were Washed With brine, dried With Na2SO4, ?ltered andconcentrated.TheremainingmaterialWaspuri?edby fractionaldistillationundervacuum togivetheamino ketone (68.0g,87%)asacolorlessoil:bp90°C./15mmHg; IR(neat) 2966,1701,1460,1366cm_l;1HNMR (CDCI3,500MHZ)6 2.70 (t, 1:67 HZ, 2H), 2.58 (t, 1:73 HZ, 2H), 2.26 (s, 6H), 1.14(s,9H);l3CNMR(CDCl3,125MHZ)6214.2(C),53.9 (CH2),45.2(CH3),43.9(C),34.6(CH2),26.0(CH3). To an ice-Water cold solution of the ketone (132 g, 0.84 mol) inethanol (70mL), NaBH4 (35 g,0.93 mol) Was sloWly added over 1 hour. After stirring continuously at 0° C. for another 2 hours and at room temperature for 2 hours, the reaction Was quenched by the addition of saturated sodium chloride (30 mL). The reaction mixture Was stirred for 30 minutes. Then, itWas ?ltered through a short pad of CeliteTM and Washed With diethyl ether. The mixture Was thoroughly extractedWithdiethylether(x3)andtheorganicextractsWere dried With Na2SO4, ?ltered and concentrated. The remaining material Was puri?ed by fractional distillation to give the A suspensionof3-pentanone(43g,0.5mol),diethylamine hydrochloride(63g,0.58mol),paraformaldehyde(16.5g, 0.55mol)andaceticacid(0.5mL)inanhydrousethanol(5040 mL) Was heated atre?ux for 1 day. The solvent Was removed under reduced pressure. The solid Was cooled in an ice Water bath and treated With an aqueous solution of 30% sodium hydroxide(30mL),folloWedbysolidsodiumhydroxideuntil thepH Was >10.ThemixtureWas ?lteredthroughashortpad of CeliteTM and Washed With diethyl ether. The mixture Was then thoroughly extracted With diethyl ether (x3), and the organic layers Were dried With Na2SO4, ?ltered and concen trated. The remaining material Was puri?ed by fractional distillationundervacuumtogivetheaminoketone(50.0g, 50 59%)asacolorlessoil:bp1000C./18mmHg; IR(neat)1713, 1461cm“;1HNMR (CDCI3,500MHZ)62.74-2.82(m,1H), 2.65-2.73 (m, 1H), 2.38-2.58 (m, 6H), 2.28 (dd, 1:60, 12.5 HZ,1H),1.04(d,1:75HZ,3H),1.02(dd,1:20,7.5HZ,3H), 0.97(t,J:7.0HZ,6H);13CNMR(CDCI3,125MHZ)6215.155 (C), 57.1 (CH2), 47.2 (CH2), 44.7 (CH), 35.2 (CH2), 15.0 (CH3),11.7(CH3),7.4(CH3). To an ice-Water cold solution of the ketone (50 g, 0.29 mol) inethanol(50mL),NaBH4 (12g,0.32mol)WasaddedsloWly over 30 minutes. After stirring continuously at 0° C. for another 1 hour and at room temperature for 2 hours, the reaction Was quenched by the addition of Water. The reaction mixture Was stirred overnight. Then, itWas ?ltered through a short pad of CeliteTM and Washed With diethyl ether. The mixtureWasthoroughlyextractedWithdiethylether(x3)and 65 the organic extracts Were dried With Na2SO4, ?ltered and concentrated. The remaining material Was puri?ed by frac 10 tional distillation to give the amino alcohol 1-diethylamino 2-methyl-3-pentanol (32.0g,64%) asacolorlessoil:bp 105° C./15 mmHg; IR (neat)3413, 3213, 2955, 2931, 1461, 1378, 1190,973cm_l;1HNMR (CDCI3,500MHZ)(tWodiastere 5H), 2.24-2.48 (m, 7H), 2.10-2.18 (m, 1 H), 1.63-1.70 (m, 1H), 1.53-1.62 (m, 1H), 1.37-1.46 (m, 1H), 1.24-1.37 (m, 2 H),0.90-1.06(m,18H),0.76(d,1:75HZ,3H),0.70(d,1:65 HZ,3H);13CNMR (CDCl3,125MHZ)(tWodiastereomers)6PDF Image | METHOD OF CAPTURING CARBON DIOXIDE FROM GAS STREAMS
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