反应详情

14.0 g (84 mmol) of 4-chloroindanone, 32.9 g (185 mmol) of 4-tert-butylphenylboronic acid, 230 ml of ethylene glycol and 38 ml of water together with 19.6 g of sodium carbonate are placed in a reaction vessel and degassed three times. A solution of 94 mg (0.42 mmol) of Pd(OAc)2 and 2.1 ml (1.26 mmol) of TPPTS in 2 ml of water is subsequently added. The resulting reaction mixture is refluxed for 5 hours. After cooling, it is extracted three times with toluene and the combined organic phases are washed with saturated NaCl solution. After drying over magnesium sulfate, the solvent is removed in an oil pump vacuum. 21.3 g (96%) of the desired product are isolated.

1. customdegassed three times
2. customThe resulting reaction mixture
3. temperatureis refluxed for 5 hours
4. temperatureAfter cooling
5. extractionit is extracted three times with toluene
6. washthe combined organic phases are washed with saturated NaCl solution
7. dry with materialAfter drying over magnesium sulfate
8. customthe solvent is removed in an oil pump vacuum