反应详情

温度

0 °C

Phosphorous oxytrichloride (0.2 mL) was added, over a period of 0.5 h, to a magnetically solution of (E)-1-[6,7-dimethoxy-3,4-dihydronaphthalen-1(2H)-ylidene]-2-(4-nitro-phenyl)hydrazine (56 mg, 0.16 mmol) in DMF (5 mL) maintained at 0° C. under a nitrogen atmosphere. The ensuing mixture was allowed to warm to 18° C. and left stirring at this temperature for 1 h then heated to 65° C. and stirred at this temperature for a further 16 h. The hot reaction mixture was poured onto crushed ice and the crystals so-formed were collected by filtration. Recrystallisation (ethyl acetate/hexane) of this material then afforded the title compound (31 mg, 54%) as orange crystals, m.p. 150° C. (with decomposition).

1. temperatureto warm to 18° C.
2. waitleft
3. temperaturethen heated to 65° C.
4. stirringstirred at this temperature for a further 16 h
5. additionThe hot reaction mixture was poured
6. customonto crushed ice
7. customthe crystals so-formed
8. filtrationwere collected by filtration
9. customRecrystallisation (ethyl acetate/hexane) of this material