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1-1: 10 ml 10 ml 1 H, 13 C NMR 20, 30 mg 1 H NMR 3 mg 20 mg ( 1 H NMR 30 mg 0.5 mg) 13 C NMR 20 mg 100 mg 1 H NMR 13 C NMR 1 H NMR ( 13 C 1 H ) 13 C NMR 20 mg (5 mg ) 2
1-1: NMR () 0.6 mlcdcl 3 5 ml NMR 3.7 ml 4 cm (3.84.2 cm ) () 3.7 ml 4 cm 5 ml CDCl 3 3
1-2: 40 mm 40 mm 40 mm 20 20 20 10 10 10 10 CENTER 10 CENTER 10 CENTER 20 20 20 4
1-2: サンプルの投入 シムの調整まで 図１ 左(ABORT)はサンプルの 強制排除ボタン 押さない 真ん中は測定中のスロット番 号 右(ADVANCE)はサンプラ ーの回転 上記写真(図 1)のように STAC MAN と書かれたオートサンプラーの上にセッ トをする 黄色いテープにスロット番号が書いてあるので サンプラーの回転 ボタン(ADVANCE)を使い 好みの番号を手前に持ってきてセットをする パソコン画面 ① 図 2: Spectrometer Control ① Sample をクリックして Sample 画面を表示させる(図 2) 5
1-2: Sample Sample State Spiner (3 ) LOCK ON IDLE( 1 4 ) Lock Control Gain 22( CDCl 3 )Reset Recall (Recet Recall 500 ) Auto Shim Z1, Z2 6
1-2: Shimming IDLE ( 5) & 10 12 2 ( ) Spectrometer Control 7
1-3: 1H NMR Experiment Experiment 1 H NMR single puls.ex2 or.exp OK ECP-500.exp, ECA-500.ex2 8
1-3: 1H NMR single_pulse.exp <Header > filename (SAKAI02090Fr6-10-1H ) auto_gain ECA-500 auto_filter force_tune 1 H NMR COSY 2 NMR <Acquisition > scans ( 8 1 mg 128 ) submit ID GO COSY 9
1-3: 1H NMR -single_pulse.exp Header filename sample_idcomment process OK auto_gain Receiver Gain() force_tune 1 H Instrument solvent recvr_gainreceiver Gain () (Receiver Gain ) NMR auto_gain 10
1-3: 1H NMR -single_pulse.exp Acquisition x_domain 1 H 19 F NMR fluorine x_offset ppm x_sweep x_offset 5 ppm x_sweep 15 ppm -2.5 ppm 12.5 ppm x_points scans x_prescans()1h 0 OK mod_return OK Pulse Pulse OK total_time x_angle x_90_width90 x_plus90 relaxation_dlay() () 11
1-4: 13 C NMR single_pulse_dec.exp Experiment 13 C NMR single pulse_dec.ex2 or.exp OK ECP-500.exp, ECA-500.ex2 12
1-4: 13 C NMR single_pulse_dec.exp <Header > filename (SAKAI02090Fr6-10-13C ) auto_gainforce_tune ECA-500 auto_filter <Acquisition > scans (( 100 mg) 64128 ( 30 mg) 256 ( 10 mg ) 100010000 ) pluse > submit ID GO 13
1-4: 13 C NMR 9 View Spectrometer Control View( 9)View Vector Process Vector ( 10, 11)4 2D NMR 10Vector 14
1-4: 13 C NMR 11: View Copy Copy (_copy) 2D Spectrometer Control STOP 15
1-4: 13 C NMR 8-1: Single_pluse_dec.exp Header filename sample_idcomment process OK sn_ratio0 SN 0 OK auto_gain Receiver Gain(1H ) force_tune 13 C Instrument solvent recvr_gainreceiver Gain (1H ) irr_noise(waltz) OK 16
1-4: 13 C NMR 8-2: Single_pluse_dec.exp Acquisition x_domain 13 C 31 P NMR phosphorous x_offset ppm x_sweep x_offset 100 ppm x_sweep 250 ppm -25 ppm 225 ppm x_points scans x_prescans() OK mod_return OK Pulse Pulse OK total_time x_angle x_90_width90 x_plus90 relaxation_delay irr_domain13c NMR 1H 1H 13C irr_offset 17
1-5: COSY COSY COSY (f2 )(f1 ) 1 H NMR 1 H- 1 H 2 () COSY 1 1 H NMR OK 18
1-5: COSY COSY 1 H NMR () Experiment ECP-500 COSY fgcosy.exp OK 19
1-5: COSY filename (SAKAI02090Fr6-10-COSY ) auto_gain force_tune <Acquisition > scans 1 OK (1 mg ) 4 16 y_points 128 256 < COSY TMS CHCl 3 20
1-5: COSY 1 H NMR 21
1-5: COSY > K Reset View Unzoom View X 22
1-5: COSY 1H NMR () Acquisition x_offset x_sweep OK x_offset x_sweep 3.8 ppm 7.9 ppm 0.15 ppm 7.75 ppm Submit COSY Spectrometer Control 23
1-5: COSY <Aquisiton > x_domaincosy Proton x_offset ppm x_sweep x_offset 5 ppm x_sweep 15 ppm -2.5 ppm 12.5 ppm x_pointsf2 2 512 or 1024 scans x_prescans() OK mod_return OK y_pointsf1 128 256 <Pulse > total_timey_points 256 5 Pluse 24
1-6: DELTA 12: Sample Slot 0 Sample window Delta Spectrometer Control 25
2-1: DEPT DEPT DEPT 13 C NMR 13 C NMR CDCl 3 CDCl 3 H DEPT CDCl 3 2 HMQC(HSQC) HMBC DEPT 13 C 13 C NMR DEPT DEPT 3 45 90 135 1 (H 3 ) 2 (H 2 ) 3 (H 1 ) 4 (H ) 135 DEPT 2 4 1 3 90 45 26
2-1: DEPT (DEPT) Experiment DEPT hp_dept_dec.exp or ex2 OK ECP-500.exp, ECA-500.ex2 27
2-1: DEPT <Header > filename (SAKAI02090Fr6-10-dept135 ) auto_gain ECA-500 auto_filter force_tune 13 C <Acquisition > scans ( 13 C NMR ( 100 mg) 32 ( 30 mg) 128 ( 10 mg ) 5005000 ) Pulse > selection angle 45[deg] submit 28
2-1: DEPT 13C NMR Pulse Pulse OK total_time x_pulsex channel 90 irr_pulse channel 90 selection_angle45 or 90 or 135 selection_pulse channel (irr_pulseselection_angle90) j_constantc-h ( OK) () C-H (Pretsch, E.; B hstructure Determining of Organic Compounds ) H CH 3 H 2 C H CH 2 OH H C CH 2 H H C O C H H C H 125 Hz 160 Hz 143 Hz 156 Hz 159 Hz 202 Hz 249 Hz irr_domain13c NMR 1H 1H 13C irr_offset 29
2-2: NOE NOE NOE 2 2.5 Å 3.5 Å 5.0 Å 2.6 Å 3.1 Å H H H 2.5 Å H H 1.8 Å NOE or NOE 1000 ROE ROESY NOE NOE(Nucleus Overhauser Effect) NOE Hα ( cis or trans NOE J ) H 3 C O O S O Ph H! H" cis 30
2-2: NOE H 3 C O O S O Ph H! H" cis H! H" CH 3 9.0 1.0 1.0 3.0 H! H! H" 9.0 1.1 CH 3 3.0 0 1.0 0.1 0 NOE H! 1 H NMR NOE 1 H NMR HαHα Hβ Hαp- Hα Hβ NOE 10%10% NOE NOE H" CH 3 31
2-2: NOE NOE 1 H NMR NOE 1 H NMR Reciever Gain 1 H NMR Delta ()Gain Value Established ( 17) 32
2-2: NOE 1 H NMR 1 H NMR () 33
2-2: NOE > K Reset View Unzoom Cursor 34
2-2: NOE Chemical Shift (ppm) 35
2-2: NOE filename (SAKAI02090Fr6-10-NOE5.3ppm ) auto_gainforce_tune <Instrument > recver_gain Reciever Gain <Acquisition > scans 32 Pulse > on_resonance irr_attenator 25 db submit, 36
2-2: NOE NOE NMR Q: NOE A D NOE D A NOE NOE Q: A irr_attenator 26dB 27dB 37
3-1: HMQC HMQC HMQC (f2 ) 1H NMR (f1 ) 13 C NMR( DEPT135) 1 H- 13 C 2 H-C 1 HMQC HMQC 1 H 13 C 140 Hz 1 H- 13 C C-H (J ) C 1 -H 1 120180 Hz C 1 -H 2 16 Hz C 1 -H 3 010 Hz C 1 -H 4 0 Hz R R H 1 H 3 C 1 H 2 H 4 R C H HMQC 1 H NMR 13 C NMRDEPT135 13 C NMR 38
3-1: HMQC Experiment ECP-500 hmqc fghmqc.exp OK 39
3-1: HMQC <Header > filename (SAKAI02090Fr6-10-HMQC ) auto_gainforce_tune <Instrument > recvr_gain 31() Instrument Spin_State SPIN OFF <Acquisition > scans 2 OK (10 mg ) y_points 128 256 40
3-1: HMQC <(f2 )> 1 H NMR 41
3-1: HMQC > K Reset View Unzoom View X 42
3-1: HMQC 1H NMR () Acquisition x_offset x_sweep OK x_offset x_sweep 3.8 ppm 7.9 ppm 0.15 ppm 7.75 ppm 43
3-1: HMQC <(f1 )> 13 C NMR View Y View Y 13 C NMR DEPT y_offset y_sweep y_offset y_sweep 20 ppm 180 ppm Submit 44
3-2: HMBC HMBC HMBC (f2 ) 1H NMR (f1 ) 13 C NMR( DEPT135) 1 H- 13 C 2 1 H 1 HMBC HMBC 1 H 13 C 8 Hz 1 H- 13 C C-H (J ) C 1 -H 1 120180 Hz C 1 -H 2 16 Hz C 1 -H 3 010 Hz C 1 -H 4 0 Hz R R H 1 H 3 C 1 H 2 H 4 R C () 1 H H ( ) 1 H HMQC 1 H NMR 13 C NMR 13 C NMR 45
3-2: HMBC Experiment ECP-500 hmqc fghmbc.exp OK 46
3-2: HMBC <Header > filename (SAKAI02090Fr6-10-HMBC ) auto_gainforce_tune <Instrument > recvr_gain 31() Instrument Spin_State SPIN OFF <Acquisition > scans 2 OK (20 mg ) (HMQC ) Submit 47
Q. A. Q. A. Q. Delta Spectrometer Control window A. Delta Delta Delta()window Spectrometer Control Spectrometer Control connect Q. Delta Fatal Delta Fatal() 48
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