Reaktion #47747

Reaktionsgleichung

acetonitrile

allylamine

aluminum

biotin-N-hydroxysuccinimide

biotin N-hydroxy-succinimide

Compound 1

biotin N-hydroxy-succinimide

→

N-Allylbiotinamide

Lösungsmittel

H2O

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeIn an argon-purged 100 ml flask
2. 2
   Waschenelution speed
3. 3
   Sonstigedetection: UV absorption (200 nm))
4. 4
   SonstigeAt 3 hours after initiation of the reaction, it
5. 5
   SonstigeThis reaction solution was used directly in the subsequent reaction

Vorschrift

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.

Quelle