核磁共振氢谱碳谱各种溶剂峰

show their degree of variability Occasionally in order to distinguish between peaks whose assignment was ambiguous a further 1 2 L of a specific substrate were added and the spectra run again Table 1 1H NMR Data protonmultCDCl3 CD3 2CO CD3 2SOC6D6CD3CNCD3ODD2O solvent residual peak7 262 052 507 161 943 314 79 H2Os1 562 84a3 33a0 402 134 87 acetic acidCH3s2 101 961 911 551 961 992 08 acetoneCH3s2 172 092 091 552 082 152 22 acetonitrileCH3s2 102 052 071 551 962 032 06 benzeneCHs7 367 367 377 157 377 33 tert butyl alcoholCH3s1 281 181 111 051 161 401 24 OHcs4 191 552 18 tert butyl methyl etherCCH3s1 191 131 111 071 141 151 21 OCH3s3 223 133 083 043 133 203 22 BHTbArHs6 986 966 877 056 976 92 OHcs5 016 654 795 20 ArCH3s2 272 222 182 242 222 21 ArC CH3 3s1 431 411 361 381 391 40 chloroCHs7 268 028 326 157 587 90 cyclohexaneCH2s1 431 431 401 401 441 45 1 2 dichloroethaneCH2s3 733 873 902 903 813 78 dichloromethaneCH2s5 305 635 764 275 445 49 diethyl etherCH3t 71 211 111 091 111 121 181 17 CH2q 73 483 413 383 263 423 493 56 diglymeCH2m3 653 563 513 463 533 613 67 CH2m3 573 473 383 343 453 583 61 OCH3s3 393 283 243 113 293 353 37 1 2 dimethoxyethaneCH3s3 403 283 243 123 283 353 37 CH2s3 553 463 433 333 453 523 60 dimethylacetamideCH3COs2 091 971 961 601 972 072 08 NCH3s3 023 002 942 572 963 313 06 NCH3s2 942 832 782 052 832 922 90 dimethylamideCHs8 027 967 957 637 927 977 92 CH3s2 962 942 892 362 892 993 01 CH3s2 882 782 731 862 772 862 85 dimethyl sulfoxideCH3s2 622 522 541 682 502 652 71 dioxaneCH2s3 713 593 573 353 603 663 75 ethanolCH3t 71 251 121 060 961 121 191 17 CH2q 7d3 723 573 443 343 543 603 65 OHsc d1 323 394 632 47 ethyl acetateCH3COs2 051 971 991 651 972 012 07 CH2CH3q 74 124 054 033 894 064 094 14 CH2CH3t 71 261 201 170 921 201 241 24 ethyl methyl ketoneCH3COs2 142 072 071 582 062 122 19 CH2CH3q 72 462 452 431 812 432 503 18 CH2CH3t 71 060 960 910 850 961 011 26 ethylene glycolCHse3 763 283 343 413 513 593 65 grease f CH3m0 860 870 920 860 88 CH2br s1 261 291 361 271 29 n hexaneCH3t0 880 880 860 890 890 90 CH2m1 261 281 251 241 281 29 HMPAgCH3d 9 52 652 592 532 402 572 642 61 methanolCH3sh3 493 313 163 073 283 343 34 OHsc h1 093 124 012 16 nitromethaneCH3s4 334 434 422 944 314 344 40 n pentaneCH3t 70 880 880 860 870 890 90 CH2m1 271 271 271 231 291 29 2 propanolCH3d 61 221 101 040 951 091 501 17 CHsep 64 043 903 783 673 873 924 02 pyridineCH 2 m8 628 588 588 538 578 538 52 CH 3 m7 297 357 396 667 337 447 45 CH 4 m7 687 767 796 987 737 857 87 silicone greaseiCH3s0 070 130 290 080 10 tetrahydrofuranCH2m1 851 791 761 401 801 871 88 CH2Om3 763 633 603 573 643 713 74 tolueneCH3s2 362 322 302 112 332 32 CH o p m7 177 1 7 27 187 027 1 7 37 16 CH m m7 257 1 7 27 257 137 1 7 37 16 triethylamineCH3t 71 030 960 930 960 961 050 99 CH2q 72 532 452 432 402 452 582 57 aIn these solvents the intermolecular rate of exchange is slow enough that a peak due to HDO is usually also observed it appears at 2 81 and 3 30 ppm in acetone and DMSO respectively In the er solvent it is often seen as a 1 1 1 triplet with 2JH D 1 Hz b2 6 Dimethyl 4 tert butylphenol cThe signals from exchangeable protons were not always identified dIn some cases see note a the coupling interaction between the CH2and the OH protons may be observed J 5 Hz eIn CD3CN the OH proton was seen as a multiplet at 2 69 and extra coupling was also apparent on the methylene peak fLong chain linear aliphatic hydrocarbons Their solubility in DMSO was too low to give visible peaks gHexamethylphosphoramide hIn some cases see notes a d the coupling interaction between the CH3and the OH protons may be observed J 5 5 Hz iPoly dimethylsiloxane Its solubility in DMSO was too low to give visible peaks NotesJ Org Chem Vol 62 No 21 19977513 Table 2 13C NMR Dataa CDCl3 CD3 2CO CD3 2SOC6D6CD3CNCD3ODD2O solvent signals77 16 0 0629 84 0 0139 52 0 06128 06 0 021 32 0 0249 00 0 01 206 26 0 13118 26 0 02 acetic acidCO175 99172 31171 93175 82173 21175 11177 21 CH320 8120 5120 9520 3720 7320 5621 03 acetoneCO207 07205 87206 31204 43207 43209 67215 94 CH330 9230 6030 5630 1430 9130 6730 89 acetonitrileCN116 43117 60117 91116 02118 26118 06119 68 CH31 891 121 030 201 790 851 47 benzeneCH128 37129 15128 30128 62129 32129 34 tert butyl alcoholC69 1568 1366 8868 1968 7469 4070 36 CH331 2530 7230 3830 4730 6830 9130 29 tert butyl methyl etherOCH349 4549 3548 7049 1949 5249 6649 37 C72 8772 8172 0472 4073 1774 3275 62 CCH326 9927 2426 7927 0927 2827 2226 60 BHTC 1 151 55152 51151 47152 05152 42152 85 C 2 135 87138 19139 12136 08138 13139 09 CH 3 125 55129 05127 97128 52129 61129 49 C 4 128 27126 03124 85125 83126 38126 11 CH3Ar21 2021 3120 9721 4021 2321 38 CH3C30 3331 6131 2531 3431 5031 15 C34 2535 0034 3334 3535 0535 36 chloroCH77 3679 1979 1677 7979 1779 44 cyclohexaneCH226 9427 5126 3327 2327 6327 96 1 2 dichloroethaneCH243 5045 2545 0243 5945 5445 11 dichloromethaneCH253 5254 9554 8453 4655 3254 78 diethyl etherCH315 2015 7815 1215 4615 6315 4614 77 CH265 9166 1262 05