Reaktion #1831591

Reaktionsgleichung

benzene

5-methyl-2-thiophenecarbonitrile

NBS AIBN

NBS

AIBN

→

5-(bromomethyl)-2-thiophencarbonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe previous reaction
2. 2
   TemperaturThe solution was refluxed for 1.5 hours
3. 3
   workup.ADDITIONafter the addition
4. 4
   Sonstigecompletion of the reaction by HPLC
5. 5
   WaschenThe reaction solution was washed with [1 L of H2O+4 L of 5% NaHCO3]

Vorschrift

1.69 kg (9.51 moles) of NBS and 156 g (0.95 moles) of AIBN were well mixed and placed in a vinyl wrapper (at this time, the previous reaction was regarded to be proceeded to 100%). The benzene solution of Example 2 was heated. The NBS-AIBN mixture was portionwise added to the heated solution at 73° C. for 40 minutes. The solution was refluxed for 1.5 hours after the addition was done. After confirming completion of the reaction by HPLC, the solution was cooled to room temperature. The reaction solution was washed with [1 L of H2O+4 L of 5% NaHCO3], and then [2 L of H2O+1 L of 5% NaCl].

Quelle