Hydrochloric Acid → HCID 178458062, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of etude MGBG (460 g) in 920 g DI water was warmed to 40°-50° C. to give a clear pale yellow solution. The mixture was cooled to 30° C. and 920 mg conc. HCl was added. A pH of 0-1 was measured with litmus paper. Isopropanol (350 g, 446 mL) was added rapidly and the mixture stirred for 1 hour at 28°-32° C. The solutions were filtered to remove insoluble material. The filtrate was added to the reaction flask and acidified further with 0.5 g of conc. HCl The isopropanol (1.84 kg) was added over 10-15 minutes to the vigorously stirred solution. The mixture was cooled to 8°-12° C. and stirred for an additional hour. The solids were collected and the cake was rinsed with 2×200 mL isopropanol. After drying in a vacuum oven at 30°-40° C. for 24 hours, the recovery was about 90%. HPLC (ETI)=0.65%, nmr (dmsod6); IR (Kbr).

Provenance & Evidence