반응 #47747

ord-995e1f5daf82450bb2905b34d4defa5a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타In an argon-purged 100 ml flask
  2. 2
    세척elution speed
  3. 3
    기타detection: UV absorption (200 nm))
  4. 4
    기타At 3 hours after initiation of the reaction, it
  5. 5
    기타This reaction solution was used directly in the subsequent reaction

실험 절차

In an argon-purged 100 ml flask, biotin-N-hydroxy-succinimide (251 mg, 0.735 mmol; Compound 1, Sigma-Aldrich) was dissolved in 26.7 ml dry DMF and mixed with allylamine (50 μl, 0.668 mmol; Nacalai Tesque, Inc., Japan), followed by stirring at room temperature with the flask covered with aluminum foil for light shielding. The progress of the reaction was monitored by C18 reversed-phase HPLC (HPLC conditions; column: μ-Bondsphere φ19×150 mm (Waters); mobile phase: 20% acetonitrile in H2O; elution speed: 10 ml/min; detection: UV absorption (200 nm)). At 3 hours after initiation of the reaction, it was confirmed that the source material biotin-N-hydroxysuccinimide was almost completely converted into Compound 2. This reaction solution was used directly in the subsequent reaction.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745417B2uspto-grants-2010_06