Hydrogen Bromide → HCID 178419707, Verbindung

Temperatur

100 °C

A solution of neomycin sulfate (20 g, 20.8 mmol) in HBr (150 mL, 48%) is stirred under reflux at 100° C. for 40 hours. The solution is concentrated to dryness at 60° C. under reduced pressure. The residue is dissolved into water (H2O) (100 mL), and activated charcoal (10 g) is added. After stirring at room temperature for 10 hours, the charcoal is removed by filtration through Celite, and the solution is concentrated to a syrup. Methanol (100 mL) is added and the mixture is stirred for 2 hours t room temperature. The solid product is filtered to give 2-deoxystreptamine hydrobromide 3 (4.1 g, 61%). Rf: 0.2 (CH3OH/NH4OH=4:1); 1H-NMR (D2O, 200 MHZ): d 1.95 (1H, ddd), 2.5 (1H, m), 3.2-3.6 (9H, m); 13C-NMR (D2O, 200 MHZ): d 40.0, 65.0, 87.2, 89.5. Ref. Georgiadas, M. P.; Constantinou-Kokotou, V. J. Carbohydr. Chem. 1991, 10, 739-746.

1. concentrationThe solution is concentrated to dryness at 60° C. under reduced pressure
2. dissolutionThe residue is dissolved into water (H2O) (100 mL), and activated charcoal (10 g)
3. additionis added
4. customthe charcoal is removed by filtration through Celite
5. concentrationthe solution is concentrated to a syrup
6. additionMethanol (100 mL) is added
7. stirringthe mixture is stirred for 2 hours t room temperature
8. filtrationThe solid product is filtered

ORD-Eintrag

ord-be16453c17f04decb0a2e70f13ec9665

Quelldatensatz

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06541456B1