Ethanol → HCID 12687119, compound

Participants

Reaction Steps

0.7g of lithium aluminum hydride was suspended in 20ml of tetrahydrofuran, to the resulting suspension was added dropwise with stirring 2.1g of 9-chloro-11-chloro-2-fluoro-10,11-dihydrodibenzo[b,f]thiepin dissolved in 10ml of anhydrous tetrahydrofuran and the mixture was stirred at room temperature for 0.5hr., further under reflux condition for 3.5 hrs., while preventing the moisture. After completion of the reaction, an excess of lithium aluminum hydride was decomposed by adding ethanol and water, and filtered off using celite. The filtrate was evaporated to obtain the residue, which was chromatographed on silica gel, eluted with chloroform, and there was obtained 1.2g(67.0% of yield) of 2-fluoro-9-chloro-10,11-dihydrodibenzo[b,f]thiepin as pale green viscous oily substance.

Provenance & Evidence