反应详情

温度

90 °C

Biphenyl 35 obtained (5.59 g) was divided into five portions (1.11 g each); then P(OEt)3 (per 7 mL) was added to each portion. The resulting mixture was subjected to argon blow in a flask, heated up to 90° C., kept at this temperature for 3 days, and cooled down. Carbazole was precipitated. Then the reaction mixture was diluted with ether; the precipitate was filtered off and washed with CH2Cl2. If the initial biphenyl remained in the filtrate (TLC monitoring, eluent: hexane-ethyl acetate, 1:1), this filtrate was evaporated and P(OEt)3 (per 1 mL into each flask) was added. The mixture was subjected to repeated cyclization for a day. The procedure repeated until the precipitation ceased and TLC data showed the absence of the initial biphenyl. Total yield of carbazole 36: 2.16 g.

1. customThe resulting mixture was subjected to argon blow in a flask
2. temperaturecooled down
3. customCarbazole was precipitated
4. additionThen the reaction mixture was diluted with ether
5. filtrationthe precipitate was filtered off
6. washwashed with CH2Cl2
7. customthis filtrate was evaporated
8. additionP(OEt)3 (per 1 mL into each flask) was added
9. customfor a day
10. customThe procedure repeated until the precipitation