Hydrochloric Acid → HCID 59753246, compound

Participants

Reaction Conditions

Reaction Steps

Next, 8 g (0.028 mol, 1 eq) of the obtained 5-bromo-5′-propyl-2,2′-bithiophene and 0.04 g (0.07 mmol, 0.0025 eq) of Ni (dppp) Cl2 were introduced into a three-necked flask, and this was flushed with Ar. To this, 100 ml of diethyl ether was added and stirred (reaction fluid α). 0.94 g (0.0385 mol, 1.38 eq) of Mg was introduced to another three-necked flask, and flushed with Ar. To this, 50 ml of diethyl ether was added and stirred. To this, a solution, of which 5.7 g (0.035 mol, 1.25 eq) of 2-bromothiophene was diluted with 50 ml of diethyl ether, was dropped. After dropping, this was refluxed for 2 hours, and was laid for cooling (reaction fluid β). The reaction fluid β was dropped to the reaction fluid α, which was cooled to 0° C. After dropping, this was stirred for 2 hours and was refluxed for 12 hours. This was cooled to 0° C., 30 ml of 2N—HCl was dropped. After dropping, the temperature was returned to the room temperature, and stirred for 2 hours. This was extracted with chloroform, water washed with Na2CO3 aqueous solution until pH is 7, and dehydrated with Na2SO4. After removing Na2SO4 by filtration, the solvent was removed. This was purified by silica gel chromatography, and specified substance of 5-propyl-2,2′:5′,2″-terthiophene (4 in the chemical reaction formula) was obtained. Yielding quantity was around 6 g, and yielding percentage was 75%.

Provenance & Evidence