反应详情

To a solution of 2[(benzyloxy)methyl-8-methyl-2,3-dihydro[1,4]dioxino [2,3-f]quinoline (0.30 g, 0.94 mmol) in CH2Cl2 (8 mL) being cooled in an ice-bath, FeCl3 (0.77 g, 4.7 mmol) was added. After 1 h, the ice-bath was removed and the reaction mixture was stirred for another 4 h. CH2Cl2 (30 mL) and 1N NaOH (25 mL) were added to result in a suspension which was then filtered. The filtered solid was washed with CH3OH (50 mL). The combined organic layers were concentrated in vacuo. Purification on SiO2, eluted with (10:1) CHCl3:/PrOH gave 0.15 g (68%) of the title compound as an off-white solid.

1. customthe ice-bath was removed
2. additionCH2Cl2 (30 mL) and 1N NaOH (25 mL) were added
3. customto result in a suspension which
4. filtrationwas then filtered
5. washThe filtered solid was washed with CH3OH (50 mL)
6. concentrationThe combined organic layers were concentrated in vacuo
7. customPurification on SiO2
8. washeluted with (10:1) CHCl3