반응 #969839

ord-9be360c63e0b4f19b270237fe455ebf1

반응 방정식

Cl.N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O
D-Glucosamine hydrochloride salt
O=C1CC(S(=O)(=O)[O-])C(=O)N1O.[Na+]
sulfo-NHS
ClCCCl
EDC
[Na+].[OH-]
Sodium hydroxide
O=CC[C@@H](O)[C@H](O)[C@H](O)CO
Deoxyglucose

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was dialyzed for 48 hours
  2. 2
    기타After dialysis
  3. 3
    온도the product was frozen
  4. 4
    기타dried

실험 절차

Sodium hydroxide (1N, 1 ml) was added to a stirred solution of EC (110 mg, 0.41 mmol) in water (5 ml). To this colorless solution, sulfo-NHS (241.6 mg, 1.12 mmol) and EDC (218.8 mg, 1.15 mmol) were added. D-Glucosamine hydrochloride salt (356.8 mg, 1.65 mmol) was then added. The mixture was stirred at room temperature for 24 hours. The mixture was dialyzed for 48 hours using Spectra/POR molecular porous membrane with cut-off at 500 (Spectrum Medical Industries Inc., Houston, Tex.). After dialysis, the product was frozen dried using lyophilizer (Labconco, Kansas City, Mo.). The product in the salt form weighed 568.8 mg. The synthetic scheme is shown in FIG. 59. The structure was confirmed by mass spectrometry (FIG. 60) and proton NMR (FIGS. 61 and 62). Radiochemical purity of 99mTc-EC-DG was 100% as determined by radio-TLC (FIG. 63) and HPLC (FIGS. 64 and 65) analysis.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08236279B2uspto-grants-2012_08