反应详情

A mixture of 1,2,3,4-tetrahydro[1]benzothieno[3,2-c]pyridine HCl (1:1) (0.02 mol), 1,1-dimethylethyl (4-chlorobutyl)carbamate (0.044 mol), Na2CO3 (0.05 mol) and KI (catalytic quantity) in 4-methyl-2-pentanone (200 ml) was stirred and refluxed overnight, then cooled to room temperature and the solvent was evaporated. The residue was washed with water and extracted with CH2Cl2. The separated organic layer was dried, filtered and the solvent evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 90/10). The desired fractions were collected and the solvent was evaporated, yielding 1,1-dimethylethyl [4-(3,4-dihydro[1]benzothieno[3,2-c]pyridine-2(1H)-yl)butyl]carbamate (intern 1).

1. temperaturerefluxed overnight
2. customthe solvent was evaporated
3. washThe residue was washed with water
4. extractionextracted with CH2Cl2
5. customThe separated organic layer was dried
6. filtrationfiltered
7. customthe solvent evaporated
8. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 90/10)
9. customThe desired fractions were collected
10. customthe solvent was evaporated