反应详情

To a solution of 78.0 g (0.4 mole) of 9-ethylcarbazole and 141 g (1.0 mole) of 4-chlorobutyryl chloride in 1 liter of methylene chloride, which has been previously chilled to 0°C, is added portionwise 127.0 g (0.95 mole) of aluminum chloride. The mixture is stirred at room temperature for 16 hours, and the resulting complex is decomposed with a concentrated hydrochloric acid-ice mixture. The organic layer is separated, washed with water, dried over magnesium sulfate and pentane added to precipitate the desired product. Recrystallization from acetone followed by a recrystallization from an acetone methanol solution results in the formation of 3,6-bis (4-chlorobutyryl)-9-ethylcarbazole, m.p. 106°-8°C; λmaxEtOH 259; and E1cm1% 1030.

1. customThe organic layer is separated
2. washwashed with water
3. dry with materialdried over magnesium sulfate and pentane
4. additionadded
5. customto precipitate the desired product
6. customRecrystallization from acetone
7. customfollowed by a recrystallization from an acetone methanol solution