Hydrochloric Acid → HCID 86742659, compound

Participants

Reaction Steps

6.6 mg (13.4 μmol) of compound IV is hydrolyzed for 2.5 hours in 0.5 ml of acetonitrile containing 76 μl of conc. HCl, to thus form compound V. The pH of the reaction solution is raised to 7.2 by addition of 500 μl of 0.1M phosphate buffer and solid NaHCO3. Gaseous nitrogen is bubbled through the solution. Then the solution is added to a slurry of 100 mg of thiopropyl Sephadex® G-50 containing 11.4 μmol of SH groups in 0.1M phosphate buffer pH 7.2. The mixture is agitated in a rotary mixer for 20 hours at room temperature. The gel is transferred to a Pasteur pipette. The reaction mother liquor is allowed to drain off, and the gel is washed with 6×1.5 ml of 0.05M phosphate buffer pH 7.4. The amount of thiopyridone that has formed is UV-analyzed in the reaction mother liquor+wash liquors. An amount of 4.45 μmol thiopyridone is detected, indicating that 4.45 μmol of compound V has been coupled to 100 mg of dry beads.

Provenance & Evidence