誘導体化試薬反応例 - Fujifilm

1 (1) GC O H C O O H N H2 TMS TMS N, O-bis trimethylsilyl trifluoroacetamide BSTFA OH CO GC/MS bromomethyldimethylchlorosilane BMDS , RCO HCl CH3OH BF3-CH3OH N, N- 1- -3-p CH3N NNHR R Alkyl Dimethylformamide dimethylacetal 1.

2 TMS 3. 4. 2. DMS 2 GC ECD ng pg XCH2Si CH3 2Cl X=Cl, Br, I HMS TFA OH NH2 TFA ECD 1 N, O-Bis trimethysilyl acetamide BSA 029-06993, 023-06991, 027-06994 1mg 2ml 50 60 C 2 l GC TMS Chlorotrimethylsilane MW bp 71 73 C/35mmHg 2 N, O-Bis trimethylsilyl trifluoroacetamide BSTFA 022-07181 1ml 4ml 90 C30 25ml 2 l GC BSA MW bp 40 C/12mmHg 3 Dimethylcholorosilane DMCS 301-60402 GC/MS MW bp 70 71 C AIMN-Acetylimidazole 3.

3 BSAN, O-Bis(trimethylsilyl)acetamide BSTFAN, O-Bis(trimethylsilyl)trifluoroacetamide CMTMS1, 3-Bis(chloromethyl)-1, 1, 3, 3-tetramethyldisilazane DMCSD imethylchlorosilane HFBIN-Heptafluorobutyrylimidazole 3. HMDS1, 1, 1, 3, 3, 3-Hexamethyldisilazane MBTFAN-Methylbistrifluoroacetamide1, 2 MSTFAN-Methyl-N-trimethylsilyl Trifluoroacetamide TFAAT rifluoroacetic Anhydride TFAIN-Trifluoroacetylimidazole 3. TMCSC hlorotrimethylsilane TMSAN-Trimethylsilylacetamide TMSDEAN-(Trimethylsilyl)diethylamine TMSIN-Trimethylsilylimidazole 5.

4 HMS 6. TFA RXH C CH3CN505099CH2Cl2503087 1CH2Cl2504083 1CH2Cl225599CH2Cl215599CH3CN254099CH2Cl2 505097CH2Cl225595CH3CN559095 2CH3CN501095 2CH3CN501099 2 O-Methyl-O-trimethylsilylmethylketene Acetal 1 p- 2 4 Chlorotrimethylsilane TMCS 200-080021,1,1,3,3,3-Hexamethyldisilazan e HMDS 309-60241 5mg HMDS/TMCS/ 2/1/10 v/v/v 5ml 50 60 C 10 N2 5ml 3 l GC TMCS HMDS HMDS MW HMDS TMCS bp 125 C HMDS 57 C TMCS 5 O-Methyl-O-trimethylsilylmethylketene Acetal136-07591 - 10mmol 5ml 12mmol 5ml 50 C 50 bp94 C/12mmHg 95%

5 TMS C MW , , , , Tetrahedron Lett., 44, 4311 1979 . 6 N-Methyl-N-trimethylsilyl Trifluoroacetamide MSTFA 538-14741, 534-14743 5 10mg 1ml 30 70 C 15 GC MSTFA TMS BSTFA BSA N-Methyltrifluoroacetamide GC MSTFA BSTFA BSA MW bp 70 C/75mmHg 1 , , 42, 103 1969 .2 , , 91, 407 1974 .3 , Chromatographia, 8 1 1975 .4 , et al., Biochemistry, 7, 749 1976 .5 , et al., Biomed.

6 Mass Spec., 8 5 1981 .6 , et al., J. Chromatogr., 241, 323 1982 .7 , et al., J. Chromatogr., 375, 285 1986 .8 , et al., , 157, 300 1986 .9 , et al., Biomed. and Environ. Mass Spec., 15, 637 1988 .7 N-Trimethylsilylacetamide TMSA 204-07101 50mg 50mg 10ml TMSA 4 MW bp 103 105 C/30mmHg , , J. Chromatogr., 26. 22 1967 .8 N- Trimethylsilyl diethylamine TMSDEA 208-07121 L- 95 C 30 25ml 2 l GC TMCS MW bp 126 127 C 1 , Chem. Ber., 94, 1876 1961 .2 , , J. Gas Chromatogr., 4, 398 1966.

7 3 , Jr.,Nature, 208, 878 1965 .4 , , Anal. Chem., 41, 1332 1969 .5 , et al., Anal. Biochem., 30, 7 1969 .9 N-Trimethylsilylimidazole TMSI 201-07091, 209-07092 TMSI 2ml 20ml 25ml 2 l GC MW bp 99 C/14mmHg 1 , , Recent Advances in Gas Chromatography., , J. A. Perry, Eds. Marcel Dekker, Inc., New York, NY 1971 .2 , , Anal. Lett., 4 1 ,41 1971 .3 , et al., Biochim. Biophys. Acta, 148, 597 1967 .4 , et al., Anal. Lett., 1, 311 1968 .5 , , , 19 9 , 1006 1973 .6 Wu,H,-L., et al., J. Chromatogr., 137, 127 1977 .7 , et al.

8 , J. Chromatogr., 151, 13 1978 . 10 N-Methylbistrifluoroacetamide MBTFA 135-07441 10mg 10mg 1ml 3 60 70 C 10 2 3 n- 10ml 2 l GC 5 10mg MBTFA 65 C 1 GC MBTFA 1,2 TFA MW pb 123 124 C 1 , J. Chromatogr., 78 273 1973 .2 , et al., J. Chrom. Sci. 15, 196 1977 .3 , et al., Proc. Nat. Acad. Sci., 83. 9784 1986 .11 Trifluoroacetic Anhydride TFAA 201-07111 50mg 2ml TFAA 25ml GC GC/MS FID ECD 12 N, N-Dimethylformamide Dimethyl Acetal040-17351, 046-17353N, N-Dimethylformamide Di-n-butyl Acetal044-17371N, N-Dimethylformamide Di-t-butyl Acetal049-18161N, N-Dimethylformamide Diethy Acetal047-17361 50mg DMF- N,N- 10ml 5 l GC DMF- DMF- -n- n.