反应详情

温度

90 °C

Compound 45 (5.0 g) was divided into five portions (1.0 g each). P(OEt)3 (per 7 mL) was added to each portion. The resulting product was subjected to argon blow in a flask, heated to 90° C., kept at this temperature for 3 days, then cooled. The carbazole precipitate was diluted with ether. The precipitate was filtered and washed with ether. If the initial biphenyl was present in the filtrate (TLC monitoring, eluent: hexane-ethyl acetate, 1:1), this filtrate was evaporated, then P(OEt)3 was added (1 mL to each flask), and subjected to cyclization for 1 day. The procedure was repeated until the precipitation ceased and TLC showed the absence of the initial biphenyl. Carbazol 46 (2.7 g) was obtained.

1. customThe resulting product was subjected to argon blow in a flask
2. temperaturecooled
3. filtrationThe precipitate was filtered
4. washwashed with ether
5. customthis filtrate was evaporated
6. additionP(OEt)3 was added (1 mL to each flask)
7. waitsubjected to cyclization for 1 day
8. customThe procedure was repeated until the precipitation