反应详情

温度

130 °C

4 g of 7-nitro-1,2,3,4-tetrahydro-1-naphthalenol [J. Pharm. Soc. Japan, Vol. 64, (1944), p. 153], 53 ml of toluene and 180 mg of p-toluene sulfonic acid were mixed together and then stirred for 2 hours at 130° C. while distilling off ≃20 ml of solvent. Then, at 20° C. 50 ml of water were added and extraction was done with ethyl acetate. The extracts were washed with a saturated aqueous solution of sodium bicarbonate, and with a saturated aqueous solution of sodium chloride, dried and concentrated to dryness. The residue was crystallized from ethanol to obtain 2.75 g of the expected product melting at ≃35° C. and after crystallizing from isopropanol melting at 37° C.

1. distillationwhile distilling off ≃20 ml of solvent
2. customat 20° C
3. addition50 ml of water were added
4. extractionextraction
5. washThe extracts were washed with a saturated aqueous solution of sodium bicarbonate
6. dry with materialwith a saturated aqueous solution of sodium chloride, dried
7. concentrationconcentrated to dryness
8. customThe residue was crystallized from ethanol