反应详情

60 ml of trimethyl orthoformate are dissolved in 400 ml of methanol, and reacted with 30 g of L-diaminobutyric acid×2 HCl at 55° C. with constant stirring. After a reaction time of 2 hours, the solvent is evaporated under reduced pressure, the crude product which remains is dissolved in 50 ml of demineralized water, and the solution is neutralized using NaOH. The compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany) using demineralized water as the eluent, and the product is dried and recrystallized from methanol. The compound obtained can be identified by means of high-pressure liquid chromatography (HPLC); (for example E. Merck, Darmstadt, Germany, LiChroCART® 125-NH2 5μ, eluent: 80% acetonitrile), and is characterized by the following 13C-NMR data: 176.8, 161.2, 53.8, 37.9, 22.0, 18.7 ppm (relative to TMS); (Galinski E. A., Pfeiffer H. P., Truper H. G. (1985) Eur. J. Biochem. 149, 135-139).

1. customAfter a reaction time of 2 hours, the solvent is evaporated under reduced pressure
2. dissolutionthe crude product which remains is dissolved in 50 ml of demineralized water
3. customThe compound is subsequently purified on an ion retardation column type BIORAD® AG11A8 (Bio-Rad Laboratories GmbH, Munich, Germany)
4. customthe product is dried
5. customrecrystallized from methanol
6. customThe compound obtained can