反应详情

2.0 g of 1-[2-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine and 2.5 g of lithium chloride are placed in a 100 ml glass vessel having a removable cover with 5 ground openings and fitted with a dry-ice condenser, thermometer, platinum sheet anode and cathode (each 2.5×2.5 cm, distance 2 cm). Subsequently, nitrogen is conducted through the apparatus for 20 minutes, the receiver is placed in a dry-ice/alcohol bath, the dry-ice condenser is charged with dry-ice and 70 g of methylamine are distilled directly into the apparatus from a pressure flask while stirring with a magnetic stirrer. Subsequently, a current of 2 amperes is applied, whereupon a voltage of 44 volts occurs and the cathode immediately becomes deep blue in color. The temperature is held at -10°. After a throughput of an amount of current of 3000 amperes (corresponding to 230% of the theoretical amount of current required for the complete conversion), the current is turned off and the solution is evaporated at 50° and under a slight vacuum. The residue is digested in hexane for a few minutes in an ultrasound bath. After filtration and evaporation, there is obtained crude 1-[2-(4,5,10,11-tetrahydro-1H-dibenzo[a,d]cyclohepten-5-yl)ethyl]pyrrolidine which is purified in analogy to the details in Examples 1(j) to 1(l).

1. customfitted with a dry-ice condenser
2. customthe receiver is placed in a dry-ice/alcohol bath
3. distillationare distilled directly into the apparatus from a pressure flask
4. customis held at -10°
5. customthe solution is evaporated at 50° and under a slight vacuum
6. waitThe residue is digested in hexane for a few minutes in an ultrasound bath
7. filtrationAfter filtration and evaporation