MAGNESIUM SILICATE (synthetic) → HCID 15617183, compound

Participants

Reaction Steps

4-Chloro-N-[2-[(2-hydroxy-2-phenylethyl)amino]-3-pyridinyl]benzamide (13.2 g, 0.036 mole) was heated at 180°-190° C. in a glass flask on a Wood's metal bath for 12 minutes. The residue was dissolved in ethyl acetate, treated with Florisil®, and filtered. The filtrate was diluted with hexanes to initiate crystallization. The solid was collected by filtration, washed with ethyl acetate/hexanes mixtures and then hexane. The solid still contained 10-15% uncyclized material, and therefore a portion of the solid (1.25 g) was heated at 180°-190° C. for an additional 17 minutes. The solid residue was recrystallized from methylene chloride/hexane and dried under high vacuum at 70° C. overnight to give 0.8 g of solid, mp. 166°-168° C.

Provenance & Evidence