Azobisisobutyronitrile → 5-(Bromomethyl)thiophene-2-carbonitrile

HRID 1744409

Reaktionsgleichung

Reaktionsgleichung von HRID 1744409
C1C(=O)N([Br:8])C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C.[CH3:21][C:22]1[S:26][C:25]([C:27]#[N:28])=[CH:24][CH:23]=1.C1C(=O)N(Br)C(=O)C1.CC(N=NC(C#N)(C)C)(C#N)C>>[Br:8][CH2:21][C:22]1[S:26][C:25]([C:27]#[N:28])=[CH:24][CH:23]=1

Komponenten

5

Edukt 4

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 3127335-Methylthiophene-2-carbonitrileHCID 86630000Nbs aibn

Produkt 1

HCID 105600165-(Bromomethyl)thiophene-2-carbonitrile

Versuchsvorschrift

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].

Aufarbeitung

  1. customthe previous reaction
  2. temperatureThe solution was refluxed for 1.5 hours
  3. additionafter the addition
  4. customcompletion of the reaction by HPLC
  5. washThe reaction solution was washed with [1 L of H2O+4 L of 5% NaHCO3]

Quellen und Nachweise

ORD-Eintrag
ord-2f748aa9f05543a6be1386a4cd7d79dc
Quelldatensatz
uspto-grants-2006_03
Patentnummer
US07015337B2

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