пример на 4-Bromo-1,2-methylenedioxybenzene
In a 500 mL-round bottom flask with reflux condenser (situated in an oil bath and with magnetic stirrer) are placed 70 g of the product from step 1 (92% pure 1,2-methylenedioxybenzene, 0.53 moles), 100 g N-bromosuccinimide and 260 mL chloroform (dry). After three hours of refluxing and stirring, the solution is cooled to room temp, and the the succinimide is filtered off with suction, and washed with 2x20 mL of chloroform. The combined filtrates are evaporated, and the residue is vacuum distilled. At 125-135°C (40 mmHg), a mixture of product and succinimide distills, which is diluted with twice the volume of diethyl ether, stored 3 hrs. over solid sodium hydroxide and washed thoroughly with water. After thorough drying over sodium sulfate, the drying agent is filtered off and washed with 20 mL diethyl ether. The ether is evaporated (rotavap), the yellow-brownish residual oil is sufficiently pure for the next step (the refractive index at 25°C is 1.583). The yield is 72 g, 67% of theory calculated to pure 1,2-methylenedioxybenzene being used.
сам лично я не возился с сукцинамидами, я не вижу смысла в этом когда бром легален и доступен везде...
я думаю прокатит в растворителе ледянка + хлороформ.. но какой выход будет не могу сказать.
мне кстати метилон из всех кетоновых стимуляторов что я пробовал больше всего понравился, чистый эмпатоген. отходняка вообще не заметил, только держит не долго.
