By Eugene V. Babaev
The writer has summarized a decade of training combinatorial chemistry into this well timed short. the forged section synthesis of unnatural heterocyclic alpha-amino acids is illustrated by means of functional examples ranging from the ABCs of peptide synthesis explored in bankruptcy one. bankruptcy is worried with the forged section synthesis that's proven on quite a few options – BillBoard, tea-bag, and Lantern units, and established on heterocyclic examples and protocols. within the 3rd bankruptcy the instruments for accelerating chemical synthesis – reliable section and liquid section – are reviewed. right here the concepts of parallel refluxing (including microwave and stream procedure) and parallel separation (filtration, centrifugation, evaporation, and chromatography) are defined. within the chapters four and five the writer is going directly to describe how the liquid part synthesis of heterocycles (reductive amination and Ugi response of heterocycles) is illustrated with using semi-automated protocols. eventually, the layout of combinatorial libraries of heterocycles is reviewed together with the unique author’s findings.
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12). The bags are again labeled. 9 mmol) of pyridine in abs. 9 mmol per one portion of resin) are added. The vials are agitated in a shaker at room temperature for 6–18 h. The bags are washed in a succession with 2 Â DCM, 2 Â DMF, 2 Â MeOH, 2 Â DCM, 2 Â MeOH, 2 Â DCM, and 2 Â hexane and dried to obtain diacyl derivatives XXVIa. Removal of one of the acyl groups: The bags with resins XXVIa are placed into a 25% solution of aqueous ammonia in DMF, agitated in a shaker at a room temperature for 18 h, and washed with 2 Â DMF, 2 Â MeOH, 2 Â DCM, 2 Â MeOH, 2 Â DCM, and 2 Â hexane to obtain monoacyl derivatives XXVIb.
Removal of N,C-Substituted Amino Acid from Support (12) Take the Bill-Board out of the rotating apparatus and unscrew caps (Fig. 2d). (13) Filter off and wash product IV with NMP (2 Â 3 ml), THF (2 Â 3 ml), and CH2Cl2 (3 Â 3 ml). (14) Mount the Bill-Board on a holder. Screw the bottom end with clean caps. Add 2 ml of CF3COOH/H2O (95:5) to each vial. Take caution! 7). ), and place in a 6-hole rack. (16) Products XVIII which are now in a solution (therefore, one should preserve the ﬁltrate) transfer to the vials.
9 mmol) of pyridine in abs. 9 mmol per one portion of resin) are added. The vials are agitated in a shaker at room temperature for 6–18 h. The bags are washed in a succession with 2 Â DCM, 2 Â DMF, 2 Â MeOH, 2 Â DCM, 2 Â MeOH, 2 Â DCM, and 2 Â hexane and dried to obtain diacyl derivatives XXVIa. Removal of one of the acyl groups: The bags with resins XXVIa are placed into a 25% solution of aqueous ammonia in DMF, agitated in a shaker at a room temperature for 18 h, and washed with 2 Â DMF, 2 Â MeOH, 2 Â DCM, 2 Â MeOH, 2 Â DCM, and 2 Â hexane to obtain monoacyl derivatives XXVIb.