反应详情

To a magnetically stirred solution of ethyl α-[3(trifluoromethyl)-benzylamino]-indole-3-acetate (1.00 g, 2.66 mmol) in 15 mL of DMF was added under nitrogen 0.112 g (2.79 mmol) of sodium hydride (60% oil dispersion). After stirring at room temperature for 10 minutes, 0.26 ml (2.79 mmol) of ethyl chloroformate was added. Stirring was continued for two hours at room temperature. At the end of this time, the reaction contents were poured into ice water, the aqueous solution extracted with ether and the ether solution washed with saturated brine and dried over anhydrous Na2SO4. Removal of the solvent in vacuo gave the crude product which was chromatographed with 80 g of silica gel using hexane-ethyl acetate (4:1) to yield 0.857 g of the title compound.

1. stirringStirring
2. waitwas continued for two hours at room temperature
3. customAt the end of this time, the reaction contents
4. extractionthe aqueous solution extracted with ether
5. washthe ether solution washed with saturated brine
6. dry with materialdried over anhydrous Na2SO4
7. customRemoval of the solvent in vacuo
8. customgave the crude product which
9. customwas chromatographed with 80 g of silica gel