The title compound (ABA-Tyr) was prepared by direct radiochemical synthesis from tritiated t&.-butoxycarbonyl-L-tyrosine and diazotised arsanilic acid followed by acidolytic deprotection and isolation by preparative high pressure liquid chromatography. The product had a specific activity of 9 Ci mmo
Synthese, resolution Optique et Radiolyse d'Acides amines A haute Activite Specifique: L-Ornithine (3H-3,4,5,5). L-Arginine (3H-3,4,5,5). Acide dl-Glutamique (3H-3,4) ET Acide dl-Glutamique (3H-3,4,4)
✍ Scribed by D. Ego; J. P. Beaucourt; L. Pichat
- Publisher
- John Wiley and Sons
- Year
- 1986
- Tongue
- French
- Weight
- 383 KB
- Volume
- 23
- Category
- Article
- ISSN
- 0022-2135
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✦ Synopsis
Ethy 2 2-acetylamin0-2-carbethoq-4-cyano-3-butene oate : -3 was prepared by condensation o f trans-I-bromo-2-cymoethylene : -2 with acetamidornalonate. -3 was catalytically reduced h t h t r i t i u m followed by 3 hydrolysis giving r i s e t o (3,4,5,5-H ) DL ornithine 5_spec. act. 103 Ci/M.
L-ormithine -S was isolated by preparative revzrsed phase HPLC on a chiral phase. From 6 , -(i(, 4 , 5 , 5 -H j DL arginine spec. a c t i v i t y : 90 Ci/mM was prepared by panidation and the 1 (+) enatiomer isolated by preparative HPLC. ethyZ sodio 3 Selective catalytic t r i t i a t i o n of 3 i n presence of t r i s ftriphenylphosphine) Rh followed by hydrolysis gave [ 3 , 4 -H J D L -g z u t h c acid spec. activ i t y 60 Ci/mM. [ 3 , 4 , 4 -H ] DL-glutamic acid spec. a c t i v i t y 90 Ci/mM was also obtained by catalytic t r i t i a t i o n of compound 1J foZlmed by hydrolysis.
3H-NMR analyses
were carried out i n each ease. Observations on the s e l f radiolysis under various storage conditions are reported.
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The molecular structure of the protonated form of tisopurine, 4-thioxo-2,5H,7H '-pyrazolo [ 3,4-d ] pyrimidinium chloride, (TPH'Cl-), was determined by x-ray di †raction methods. The crystals are monoclinic, C 5 H 5 N 4 SCl space group with a = 7.332(5), b = 10.911(9) and c = 9.423(8) b = 104.99(6)Ä
## Abstract Three novel chiral packing materials for high‐performance liquid chromatography were prepared by covalently binding of (2S)‐N‐(3,5‐dimethylphenyl)‐2‐[(4‐chloro‐3,5‐dinitrophenyl)carbonylamino]propan‐amide (**7**), (2S)‐N‐(3,5‐dimethylphenyl)‐2‐[(4‐chloro‐3,5‐dinitrophenyl)carbonylamino]