HCID 178460303, compound → HCID 178512720, compound

Participants

Reaction Conditions

Reaction Steps

57.9 g of N-[[[2-[[[2-[(diaminomethylene)amino]-4-thiazolyl]methyl]thio]ethyl]amino]methylene]-4-bromo-benzenesulfonamide isopropanolate are dissolved in 87 ml of methanol at a temperature ranging between 40 and 50° C. The resultant solution is allowed to stand till a certain degree of turbidness fades away, then filtered and poured onto 550 ml of water at 0-5° C. for 4 hours under energic stirring. After the addition is completed, the mixture is stirred for further 4 hours at 0-5° C. and filtered. The filtrate is washed with abundant water and dried in vacuo at a temperature below 30° C. to yield 49.9 g of ebrotidine Form A.

Provenance & Evidence