Acetone → RAS-2410 hydrochloride

Participants

Reaction Conditions

Reaction Steps

A second reaction vessel was charged with aqueous hydroxylamine (50%, 42.8 kg, 647 mol) and THF (40.0 L). The above prepared solution of (E)-3-[1-(4-dimethylaminomethyl-benzenesulfonyl)-1H-pyrrol-3-yl]-acryloyl chloride hydrochloride was added at 18-30° C. over a period of 2-4 h. After stirring for 20-40 min, acetone (47.6 L, 647 mmol) was added at 17-25° C. within 45-90 min. The reaction mixture was stirred for 30 min and acetonitrile (570.0 L) was added over a period of 1-2 h. The suspension was stirred at 17-25° C. for at least 4 h, cooled to 5-13° C. and stirred for 1-2 h. The solid was centrifuged and was used without further drying in the subsequent free basing step.

Provenance & Evidence