Diisopropyl Ether → HCID 86626445, compound

Participants

Reaction Steps

4.86 L of ethyl acetate was added to 345 g of benzyl (3S,4R)-3-cyclopropylaminomethyl-4-hydroxypyrrolidine-1-carboxylate (1.20 mol) to dissolve the compound. While this solution was stirred, 1.04 L of a 10% hydrogen chloride methanol solution was added at an internal temperature of 21° C. Following the formation of crystals (internal temperature of 20° C.), the mixture was kept stirred for 15 minutes. Subsequently, 9.72 L of diisopropyl ether was added slowly and the mixture was further stirred for 30 minutes. The resulting crystals were collected by filtration, washed with 0.52 L of ethyl acetate, and drained for 30 minutes. The product was then dried by air-blowing at 60° C. for 4 hours to give 350 g of the title compound as white powder crystals (90% yield in the 2 steps).

Provenance & Evidence