2,5-Dimethylpyridine synthesis
- Product Name:2,5-Dimethylpyridine
- CAS Number:589-93-5
- Molecular formula:C7H9N
- Molecular Weight:107.15
Yield:589-93-5 84%
Reaction Conditions:
with Raney nickel at 180; for 0.5 h;Flow reactor;Green chemistry;regioselective reaction;Concentration;
Steps:
3.2. General Flow Procedure for the Synthesis of 2-Methylpyridines
General procedure: The continuous flow system was set up as described in Figure 1 by using either a Waters 515 pump or Vapourtec R2 pumping module to progress 1-propanol through a stainless steel column (150 × 4.6 mm) packed with 5.5 g of Raney nickel. Initially, while a 0.05 M solution of the respective pyridine was prepared in 5 mL of 1-propanol, the flow rate was set to 0.3 mL/min and the catalyst column was heated in a sand bath to >180 °C for 30 min. The flow rate was then set to 0.1 mL/min and the sample was placed in a 5 mL sample loop and introduced into the reaction stream. The dead volume had been estimated at ~1 mL (~2.5 mL max theoretical, 150 × 4.6mm cylinder) giving a ~10 min residence time: however, the sample was collected for 30 min to ensure complete collection. The solvent was evaporated to yield a product that was of sufficient purity for further use.
References:
Manansala, Camille;Tranmer, Geoffrey K. [Molecules,2015,vol. 20,# 9,p. 15797 - 15806]
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