æ©æ¬,è. ãã PPM ä½ç£å ´å´ ï¼é«å¨æ³¢æ°å´ï¼ é«ç£å ´å´ ï¼ä½å¨æ³¢æ°å´ï¼ X: é»åå¸å¼åº X C H X: é»å ⦠ããããã¤ï½¡ ãã®ä»ã®æ ¸ç¨®ï½¤ä¾ãã°-3Cã19Fã®æ ¸ç£æ°é®è½ ã«ã¯ç¬¬äºé
ã®å¯ä¸ãç¡è¦ã§ããªã。ããã¯æ¸©åº¦é ä¾åå¸¸ç£æ§é
(TIP)ã¨å¼ã°ã、pé»åãdé»å㪠ã©ååæ ¸ã®ã¾ããã«å¯¾ç§°ã§ãªãåå¸ããããé»å ã«ããé®è½ã§ãã。 C,p=Cï½¥Pï½¥(AE)-Iï½¥(r3) åºãçµåãã¦ããå ´åããããã®ç½®æåºã¯é»åä¾ä¸åºã¨ãªãã¾ãã åå¤å±,ä¸é. é¢é£ãã¼ã¸. ä¸ã¤ã«å¯¾å¿ãã¦ä¸ãããã¦ããæ
å ±ã¯æ¬¡ã®ã¨ããã§ãã deptãæ¸¬å®ããã¨ãcã¨çµåãã¦ããhã®æ°ã夿ããã âdeptã®è¦æ¹. ããã¯å¤é¨ç£å ´ã®å¤§ããã«ããããåãå¤ã¨ãªãï¼å¾è¿°ï¼ã ã» é½åã¾ãã¯ä¸æ§åã奿°ã®æ ¸ç¨®ã¯NMRå¿çï¼ 1 H, D, T, 14 N, 19 F, 31 P, 13 C ã» é½åã䏿§åãã¨ãã«å¶æ°ã®å種ã¯NMR䏿´»æ§ï¼ 12 C, 16 O éã¯ãããã«ã ä¸ã®å種溶åªã®13cã®ãã¼ã¿ . ããã®äºæ¸¬ ã»ã¾ãã1H NMRããäºæ³ãããæ§é ã¨çç¾ããªããã¨ã確èªã ã°ãã«ã®æ¬æ°ã¨ååç©ã®cã®æ°ãåã£ã¦ãããã¨ãããã¨ãè¦ãã®ãã»ã¼å
¨ã¦ã§ãã 13c-nmrã®æ¸¬å®. ãã. Molecular formula: C 8 H 10 N 4 O 2. (x10,000) N N N N O O CH 3 H 3 C CH 3 Caffeine. æ°¸ç°,親æ¸
. 1 H NMRï¼ 1 H NMRã¯ãååä¸ã«åå¨ããæ°´ç´ ⦠ããä½ç½®ãä½µè¨ã,æ´ã«ä¸ç½®æä½,1,1-äºç½®æä½,1,2 ããå¤ã帰å±ããªããã 35.0 40.0 45.0 50.0 55.0 60.0 65.0 70.0 75.0 80.0 85.0 90.0 95.0 100.0 105.0 110.0 115.0 120.0 125.0 130.0 135.0 140.0 145.0 150.0 155.0 160.0 165.0 170.0 175.0 180.0 185.0 190.0 195.0 m/z 0.00 0.25 0.50 0.75 1.00 Inten. å¼ç¤¾ã§æ¨æºçã«è¡ã£ã¦ããnmrã«ãã1次æ§é ã®è§£æã¯1次å
1 hã 13 c nmr ã®æ¸¬å®ã次㫠1 hâ 13 c hsqcã 1 hâ 1 h cosyãæå¾ã« 1 hâ 13 c hmbcã 1 hâ 1 h tocsyã§ãã試æéãéãããå ´åã«ã¯æãæåº¦ã®é«ã1次å
1 h nmrã¨ãã® 1 hæ ¸ã®ã¿ã§æ¸¬å®å¯è½ãª 1 hâ 1 h cosyã 1 hâ 1 h tocsyã®ã¿ã測å®ãããã¨ã ⦠ããç¸é¢ï¼åèï¼ 10 9 8 7 6 5 4 3 2 1 0 ppm c=c c-o c-n ch=o âchâ å¶å¤,è¬èµ. ç£å ´h'ãçããã ãã£ã¦ãååæ ¸ã«ãããå®éã®ç£å ´h㯠æ¸ç°,æä¸. ããã¨æ¯ã¹ã¦ã¨ã¦ãç¯å²ãåºãããã®ãããªçç±ãããããããã¨ãåãæ©æ¢°ã§æ¸¬å®ããã¨ãã¦ã 1 H㨠13 Cã®ã¹ãã¯ãã«ãéãªããã¨ã¯ãªãã ã¹ã㳠⦠ãã ææ°(104å)ã®å½è©¦ã¯æ°ãµã¤ãã§è§£èª¬ãã¦ãã¾ãã ãã ãäºæ¸¬ã§ããã°ä¾¿å©ã§ããã¨ãã観ç¹ããç½®æåºã®å½±é¿ 度ãã¨ããã ãµã³ãã«é1 mg以ä¸ã§ãokã ã»ãã¼ã¯é¢ç©ã«å®éæ§ãããï¼ãããã³ã®åæ°ï¼ã®æ¯çï¼ãåããã ãã 並åã¿ã¤ãã« (alternative) Graphic renpresentation of C-13 NMR chemical shifts (X) : The chemical shifts for methylene, methyne and quaternary carbons èè
(creator) ç°ä¸,èª ä¹. ã°ãã«å士ã®éãªããããªãå°ãªããªã£ã¦ããã æ¦æ¨,æ¸
. ãã ï¼ppmï¼ tms ï¼åºæºãã¼ã¯ï¼ si(ch3)4 0 ã¢ãã³ r-nh- ar-nh- 1.0-3.3 3.0-5.0 第ä¸ç´ã¢ã«ãã« ch3-r 0.7-1.3 ã¢ã«ããã« -cã²c-h 2.3-3.0 ããç¯å²ã¯0ã240ppmã§ããã NMRã¹ãã¯ãã«ãå¾ãããã«ã¯ããã¼ãªã¨å¤ææ³ãç¨ãããã¨ãã§ãããããã¯æº¶åªãã¼ã¯ã観å¯ãããé«éããã»ã¹ã§ãã 1 h nmrã¨13 c nmrã®éã å®ç¾©. 1hnmr; ææ©åå¦ãã¼ã¿éããããã¼ã¸; åèæç®ãé¢é£æ¸ç±ããããããªæ¬ åå¦è
åãã®æ¬. dept.