TLC - chem.ryukoku.ac.jp

1 1 1 1. 2 2. 3 3. work up 4 4 4 5 6 4. TLC TLC 6 7 TLC 8 crude TLC 8 TLC 8 TLC 5.

2 9 9 9 9 10 10 11 6. 11 11 7. 12 TLC 13 13 13 13 14 14 TLC 5 cm 5 cm 14 15 8.

3 NMR 15 16 16 16 16 17 18 18 18 9. Chem Draw 19 10. 19 11. 19 12. 20 23 27 29 13.

4 29 2 1. 1. B 6mm 35 30 50 2. 2008 4 1 5 3. 100 YN100 4. 2 TLC 5. ID NMR,MS,EA TLC 1H-, 13C-, 31P-NMR . NMR Lot TK TK220 1H NMR HMR 220-1, HMR 220-2, HMR 220-3, CMR 220-4.

5 %y 00 mg .. ppm ppm . ACS MS . Lot ExactMass 4 ChemDraw Analysis .. NMR 3 2. Chem Draw 5 1. TI624 2.

6 3. 4. 2008 4 1 08 4 1 5. recrystaln from ethanol TI624 08 4 1 recrystaln from EtOH 4 3. work up crude ( ) ( ) ( ) 2 ( ) crude Crude Crude ( ) workup ( ) ( )

7 1 1 ( ) extraction 3 ( ) brine brine brine brine ( ) Na2SO4 ( ) Na2SO4 ( ) workup ( ) ( ) 3 ( ) Brine 1 ( ) Na2SO4 ( ) Na2SO4 ( ) 5 workup ( ) ( ) ( ) 3 brine ( )

8 Na2SO4 6 3 1 10 4. TLC TLC TLC TLC 20 cm 20 cm 60 F254 Merck SiO2 TLC 2 cm 5 cm, 5 cm 5 cm ( ) TLC TLC ( ) 240 ( ) ( ) ( ) ( )

9 ( ) 10 15 ( ) ( ) 1 2 3 7 i) ( ) ii) (HI) 2 ( ) 5 6 ( ) ( ) ( ) 45 ( ) (LOW) iii) ( ).

10 8 TLC ( ) ( ) TLC 2cm X 5 cm S A R Mi Mixture 7 mm R 2 2 h 30 h ( ) 1 1 ( ) ( ) Rf TLC Rf crude TLC ( ) Crude 1H NMR ( ) NMR NMR NMR TLC ( ) NMR TLC ( ) TLC S A C crude Mi Mixture ( ) Crude 1 Rf TLC ( ) A B 3 ( ) 3 Rf A B ( ) 3 Rf A B ( ) 3 Rf A B ( )