Диссертация (1150167), страница 18
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Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2lC3F3Cl6.8(ppm)3.2Рис. 27. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2n124-70.5120-70.5255-70.3336-70.3471158.7074170Cp-165160155Ci-150132145Co-140135(ppm)1306.01255.81205.6(ppm)C1F3(ppm)1155.4H3COC F3Co-Cм-110 105(ppm)55.181455.13866.25.2H1005.0C395Hb4.8904.6H3CO2C85803.31203.07811.00000.9910(ppm)4.44.2126Cм-75Ha(ppm)4.0Ci-114(ppm)703.860(ppm)653.6600.40523.31203.0781Integral1.00004.88804.87594.86254.84864.83593.86073.84053.78633.77246.87276.85566.84386.82727.25987.25257.23547.22227.20563.78633.77244.46044.44404.88854.87594.86254.84864.8359CF360.523660.284560.049059.809955.199255.181451.25956.460.523660.284560.049059.80996.60.9910Integral6.87276.85576.84386.82727.25257.23547.22227.2056Ha77.00006.8114.0995113.89617.0114.0995113.89617.2122.88906.9125.11947.4132.2995131.7820129.7015128.8451127.3498125.1194122.8890120.67297.0(ppm)128.84517.67.1129.70157.24.31844.34557.3131.7820132.2995158.7074IntegralH3COHbClH3COOCH3OCH3HbHa6.83.8(ppm)(ppm)3.4553.2Рис.
28. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2pC1F3HCl1CH3CH355.2(ppm)C2CH3130C3C25045Рис. 29. Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2p125190MeO(ppm)180170OMe132.0(ppm)126160150140124(ppm)130(ppm)120110122(ppm)1005.0(ppm)4.0903.0CF3Д2112(ppm)8070602.0C260.0(ppm)55.5(ppm)5040302051.598551.4201H3.11993.11973.00534.45204.43554.41834.86314.8502Д155.195755.1778Ha55.920155.820255.795260.512960.473760.273860.241760.034760.006259.795659.767155.920155.820255.795255.195755.177851.598551.42011.0000(ppm)3.00533.11973.11991.0000(ppm)60.034760.006259.795659.76716.0111.3481111.1803111.02331.00046.85626.84486.83746.82766.82076.80816.78886.76117.26007.23857.22597.2090CF3HaCl60.512960.473760.273860.24172q1.00046.8(ppm)112.3152Cl114.0852113.8604C27.0119.9021C3Hb120.62656.00362.0024MeO121.32958.0122.84629.06.00362.00246.9125.8081125.0766MeO158.7323148.9828148.7973148.2513132.7242132.1211132.0568131.5073129.7408128.8272127.3070125.8081125.0766122.8462121.3295120.6265119.9021114.0852113.8604112.3152111.3481111.1803111.0233Integral7.2(ppm)127.3070H131.507310.0132.1211132.0568132.7242148.2513148.9828148.79733.78773.77313.85733.84133.8341MeOД22qOMe(ppm)1.0Рис.
30. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2qC1F3HC3Д151.5(ppm)(ppm)10Рис. 31. Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2q12603.85733.84133.83413.78773.77314.45204.43554.41834.86314.85027.26007.23857.22597.20906.88556.88226.87326.85626.84486.83746.82766.82076.80816.78886.761110.09.08.07.0(ppm)6.0-70.5(ppm)H5.00(ppm)5.0(ppm)1.2818-70.04.55524.5363-69.51.0000-69.01.00005.01184.99834.99334.98444.97944.96584.95234.55524.5363-68.51.00271.00274.99834.99334.98444.97944.96584.95237.35227.34377.32137.26007.24457.2390-68.07.26007.24457.23907.35227.34377.32131.04701.0000Integral-70.5425-70.5560-70.3723-70.3858Cl-71.04.0-70.5425-70.5560-70.3723-70.3858CF31.04701.0000MeO1.12399.0259-67.59.02591.1239IntegralMeOД2Д12qOMe-70.4(ppm)-71.5-72.0Ha3.0-72.5Ha-73.02.0-73.51.0-74.0Рис. 32.
Спектр ЯМР 19F (470 MГц, CDCl3)соединения 2qCF3HbBr2r(ppm)0.0Рис. 33. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2r127C3127.4144127.3716PhC250.411650.176149.940549.7050HBr2r120.6156С2С3СFС11601122.8355128.0(ppm)125.0554129.0126.804150.411650.176149.940549.7050127.7713128.3495H128.7528128.567253.570177.0000140.5801140.1162128.7528128.5672128.3495127.7713127.4144127.3716126.8041125.0554122.8355120.6156C1F3Ph150140130126120124122(ppm)110100С212090(ppm)51807060504050(ppm)304920-63.2622-63.2757Рис. 34. Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2rPhPh-61.8-62.0CF32rBr-62.2-62.4-62.6-62.8-63.0-63.2-63.4(ppm)-63.6-63.8-64.0-64.2-64.4-64.6-64.8-65.0Рис. 35.
Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2r128(ppm)200(ppm)190180142(ppm)170160150140129.0128.0(ppm)114(ppm)126130120110100(ppm)5.0(ppm)PhHC1F3C3H3CO124(ppm)90C280703.78343.7619Д24.50(ppm)4.03.0C1F3H(ppm)602.0(ppm)5040302049.853450.974050.742050.545750.510150.317450.271050.08544.50564.49464.48794.47532t55.192152.890352.401450.974050.742050.545750.510150.317450.271050.085449.853430.87554.95(ppm)3.05881.0014Hb3.05881.00141.00001.00004.94064.92704.92274.90894.89514.88106.86896.85156.83026.81287.29657.28767.26007.25197.23457.22047.2030Br52.890352.401455.19216.0122.81412.03422.03423.02324.1439IntegralMeO125.05167.0114.1316113.89618.0114.1316113.89619.0127.2891127.260610.07.0(ppm)127.67814.14393.02327.2128.2027129.5588128.9557128.8593128.7130128.5596128.5060158.8073158.7930140.8999140.4966132.6028132.2031129.5588128.9557128.8593128.7130128.5596128.5060128.2027127.6781127.2891127.2606125.0516122.8141Integral7.4132.6028132.2031140.8999140.4966158.8073158.7930HaCF3HbСН3Д1acetoneHa6.8(ppm)1.00.0Рис.
36. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2tBr2tC2Д2Д151.0(ppm)122100Рис. 37. Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2t1292.17094.95394.94064.92704.92274.90894.89514.88104.50564.49464.48794.47533.78343.76197.32867.32057.31637.29657.28767.26007.25197.23457.22047.20306.86896.85156.83026.81289.07.08.06.97.06.0Hb4.9(ppm)5.0(ppm)-68.2Ha4.5(ppm)4.03.03.7712-68.01.84863.7897-67.8Integral-67.6(ppm)1.1197-67.43.78973.7712-67.24.49624.47864.46364.89694.88304.86914.85204.83824.49624.47864.4636-67.01.00001.00184.89694.88304.86914.85204.8382-66.82.99947.1(ppm)-66.61.00007.2-66.41.00187.3-66.26.87706.85976.84156.82427.31157.29447.27737.26007.25667.23937.22707.22157.20957.20407.18747.16986.87706.85976.84156.8242-66.02.07733.58547.26007.25667.23937.22707.22157.20957.20407.18747.1698-65.82.07731.96731.00001.1384IntegralMeO1.96733.5854IntegralCF3BrД12tД2-68.4-68.6-68.8Д1Cl2.0-69.0-69.2Рис.
38. Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2tД2H3COHaCF3HbBr2w3.78(ppm)1.0Рис. 39. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2w130-67.7100-67.7262-67.4560-67.4695-67.5911-67.6046(ppm)190-67.00(ppm)180129.5170-67.10129.0(ppm)160Cl-67.20133.2(ppm)150140-67.30130-67.40120-67.50110-67.60(ppm)1002wC1F3128.590-67.70OCH3124(ppm)(ppm)80-67.807060-67.90(ppm)50-68.004030-68.102049.864149.832049.6286ClC250.531550.331650.299550.096150.0640355.2206128.8986128.7630128.7202129.0342129.4339129.7122C51.905451.8090114.2351114.0352131.6678132.0247H120.4802122.6999124.9196127.1393133.2238133.1917138.9835139.2191158.9357(ppm)114.2351114.0352158.9357139.2191138.9835133.2238133.1917132.0247131.6678129.7122129.4339129.0342128.8986128.7630128.7202127.1393124.9196122.6999120.480255.220651.905451.809050.531550.331650.299550.096150.064049.864149.832049.6286H3COC 1 F3HBrС1С2Д1(ppm)10Рис. 40.
Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2wH3COCF3Д1+ Д2Br2w-68.20Рис. 41. Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2w131Д2(ppm)49.5(ppm)0200190180170160150140126130120110100(ppm)3.19373.08125.0(ppm)4.0Br(ppm)1249080703.77034.47834.46043.7888(ppm)3.08121.00001.13062x3.1937(ppm)3.0602.0H3COC1F3122(ppm)(ppm)5040302050.40666.01.00001.13064.91704.90354.88954.88564.87194.85776.87916.86176.84236.8251Br50.6385H2.18452.10212.10212.18457.26007.25057.23317.21777.2005CF350.8705C1F355.163651.702051.098950.870550.638550.40667.051.098951.7020C255.1636C34.90(ppm)122.81768.0114.0567113.86399.0132.9062132.5315129.3589128.7309127.2570125.0373122.8176120.75502.01432.11247.2(ppm)125.0373127.2570H2.11242.0143MeO114.0567113.8639158.6681Integral3.78883.77034.91704.90354.88954.88564.87194.85774.47834.46047.26007.25057.23317.21777.20056.87916.86176.84236.8251MeO(ppm)1.00.0Рис.
42. Спектр ЯМР 1H (500 MГц, CDCl3)соединения 2xH3CO2OCH3C3C2114(ppm)51.0(ppm)C110Рис. 43. Спектр ЯМР 13C (125 MГц, CDCl3) соединения 2x132010.09.08.0Ha8.07.0CF3HbF7.06.0Hb5.4(ppm)6.05.0(ppm)3.07283.18753.10811.00004.45654.44004.4255OMeCF3(ppm)5.0(ppm)4.04.03.78813.77003.85633.83653.8327Д13.10813.07283.18751.00002y4.46054.44744.41744.40439.01.000010.00.9934MeOД14.46054.44744.41744.4043BrCF3HaBr2y1.00000.9950MeO5.47095.45885.44665.43425.42215.38015.36825.35585.34345.3312Hb5.52982.0755MeO5.47095.45885.44665.43425.42215.38015.36825.35585.34345.33127.36657.34157.33587.31657.28107.26817.2600Integral1.56362.17163.86203.85633.83653.83273.78813.77004.45654.44004.42554.87294.86127.26007.24337.22597.21237.19526.87036.85366.83506.81836.79596.77886.7475OMe0.995010.594IntegralMeOД1Д2Д2HД2aceton3.80(ppm)HРис.
44. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2yHa2z4.4(ppm)3.02.03.02.01.01.00.00.0Рис. 45. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2z13310.09.08.07.0-1306.0-140(ppm)5.0(ppm)-150Hb5.45.3(ppm)4.01.2885-1204.44554.43274.40124.3887-1104.44554.43274.40124.38875.44595.43445.42215.40935.39655.38395.35565.34365.33135.31875.30595.29367.34987.33657.32277.30487.2829-1001.00000.88325.39655.38395.35565.34365.33135.31875.30595.29367.34987.33657.32277.30487.2829-901.00009.3990Integral-800.88329.3990Integral-70-200.2603-200.2820-200.2847-200.3036-200.3090-200.3333-200.3576-200.3819-200.4062-200.4306-200.4549-200.4792-76.2997-76.3132-76.3240-76.3375-76.2997-76.3132-76.3240-76.3375-200.2603-200.2820-200.2847-200.3036-200.3090-200.3333-200.3576-200.3819-200.4062-200.4306-200.4549-200.4792CF3F2z-200.2(ppm)-160-170HaCl3.0-1807.32.0-200.4-1901.0-200.6(ppm)-200Рис. 46.
Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2zCF 3HbFHa2zb(ppm)(ppm)greace0.0Рис. 47. 1H Спектр ЯМР соединения2zb (500 MГц, CDCl3)13410.09.08.0-957.0-100-1056.0-110(ppm)Hb5.4(ppm)4.4(ppm)5.0(ppm)3.10243.78633.7824-137.2-1153.78633.7824СF30.9998-90-137.2175-137.2418-137.2661-137.2904-137.3148-137.3391-137.3614-137.3877-137.4120-137.4343Д24.42454.41044.38174.36761.0000СF33.10247.0(ppm)-855.43065.41865.40615.39295.38045.34005.32775.31535.30235.28984.42454.41044.38174.3676-801.2935IntegralСF-137.6-1204.0-138.0099-138.0322-138.0565-138.0788-138.1031-138.1274-138.1517-138.1760-138.1983-138.2206Cl0.99981.00435.41865.40615.39295.38045.34005.32775.31535.30235.28987.34677.34077.33377.33177.26357.24596.88286.87526.86576.8578-76.21.00437.26.88286.87526.86576.8578-752.06391.22106.28517.33377.33177.26357.2459Д12.06396.28511.2210Integral-70-76.3166-76.3288-76.3409-76.3531-76.1910-76.2031-76.2153-76.2275-76.1910-76.2031-76.2153-76.2275-76.3166-76.3288-76.3409-76.3531-137.2661-137.2904-137.3148-137.3391-137.3614-137.3877-137.4120-138.0565-138.0788-138.1031-138.1274-138.1517-138.1760-138.1983CF3F2zbД1Д2(ppm)-138.0-1253.0-138.4(ppm)-76.4СF-1303.80-1352.0-140-145Д1HaHaMeO1.0-150Рис.
48 Спектр ЯМР 19F (470 MГц, CDCl3) соединения 2zbД2CF3HbF2zd6.8a(ppm)H0.0Рис. 49. Спектр ЯМР 1H (500 MГц, CDCl3) соединения 2zд135(ppm)200190180131.0170160150140124130122(ppm)120119.42036.0130.0(ppm)1105.4(ppm)5.0(ppm)91100(ppm)906.05941.0000(ppm)(ppm)1.00000.94116.05944.44.0807055.209955.181448.911348.757991.078290.824990.575190.321789.558089.304689.054888.80150.94114.09574.3996Integral4.36594.35364.32184.30925.33455.32205.28055.26735.25575.24345.23076.86436.85047.25397.23757.2215Hb3.0H3CO55.2(ppm)605048.911348.757912055.209955.1814С1F3114.2244113.99247.0121.6650121.45444.09574.39966.889.558089.304689.054888.8015123.9132123.69918.0125.9473131.3645131.3324130.3118129.7551129.0949126.1614125.9473123.9132123.6991121.6650121.4544119.42037.0129.0949158.7645158.74669.0129.7551130.3118131.3645131.3324Integral7.291.078290.824990.575190.3217158.7645158.74663.7801H3COHaHaH40CF3HbFH3CO2ze3.80(ppm)2.01.0C3C230200.0Рис. 50.
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