Hydrochloric Acid → HCID 86670069, compound

Participants

Reaction Conditions

Reaction Steps

2-(4-benzylamino-3-trimethylsilanylethynyl-phenyl)-ethanesulfonic acid methylamide (100 g) was dissolved in ethanol (1000 ml) at 25° C. and cooled to 15-20° C. Potassium hydroxide (20 g) was added slowly maintaining temperature below 25° C., stirred for 2-3 hours and cooled to 10-15° C. pH of the reaction mixture was adjusted to 5 with 10% dilute HCl and concentrated under vacuum below 40° C. to obtain a residue. The residue was dissolved in water (300 ml) and extracted with dichloromethane (2500 ml). The organic layer was washed with water and concentrated under vacuum to obtain a residue. The residue was treated with heptane (400 ml) to obtain a solid which was filtered and dried under vacuum at 50-55° C. for 12 hours. (Yield: 75 g, HPLC Purity: 98%)

Provenance & Evidence