反应详情

A mixture of 1,2,3,4-tetrahydro-[1]benzothieno[2,3-c]pyridine (0.02 mol), Na2CO3 (5 g), KI (0.1 g) and 4-chlorobutanenitrile (0.025 mol) in acetonitrile (50 ml) and methylbenzene (150 ml) was stirred and refluxed overnight, then cooled, filtered and the filtrate was evaporated. The residue (oil) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2). The pure fractions were collected and the solvent was evaporated, yielding 5.2 g of 3,4-dihydrobenzothieno[2,3-c]-pyridine-2(1H)-butanenitrile (interm. 6).

1. temperaturerefluxed overnight
2. temperaturecooled
3. filtrationfiltered
4. customthe filtrate was evaporated
5. customThe residue (oil) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 98/2)
6. customThe pure fractions were collected
7. customthe solvent was evaporated