Methyl iodide → HCID 88411977, compound

Participants

Reaction Steps

1.1 g of 2-morpholinomethyl-6-n-propyl-8alpha-ergolinylamine (3 mmol) is formylated as described in example 4, then mixed, in 50 ml of tetrahydrofuran, with 2 ml of methyl iodide and stirred for 20 hours at room temperature. Then it is cooled in an ice bath and mixed with diisopropyl ether for completion of the crystallization. The crystals are isolated and dissolved in 30 ml of methanol. At the same time, a methylate solution, in which the solution of the quartenary salt is instilled at 0° C., is prepared from 230 mg of sodium (10 mmol) in 20 ml of methanol. After 15 minutes stirring at 0° C. and 30 minutes at room temperature, ice is added and extraction is performed with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed on silica gel with dichloromethane and methanol, yield 470 mg (48% of theory).

Provenance & Evidence