HCID 25113700, compound → HCID 25113699, compound

Participants

Reaction Conditions

Reaction Steps

(S)-1-(4-Chloro-5-isoquinolinesulfonyl)-3-(methylamino)pyrrolidine (150 g) obtained in Example 1 was suspended in 2-propanol (2400 ml), and the suspension was warmed to 61.5° C. to dissolve the compound. This solution was filtered by using a membrane filter (internal diameter: 90 mm, ADVANTEC PTFE, 0.2 μm), and the filtrate was added dropwise with 300 ml of a mixed solution of hydrochloric acid (35%, specific gravity: 1.18, 48.0 g, Kanamori Industry) and purified water (261.4 ml, Fukuju Pharmaceuticals) with maintaining the filtrate at 55° C. The mixture was stirred at 55° C. for 44 minutes, then cooled to 2.0° C. over 2 hours and 11 minutes, and further stirred for 1 hour and 28 minutes, and then the deposited crystals were separated by suction filtration using a Buchner funnel (internal diameter: 150 mm, filter paper: No. 5C). The pale brown wet crystals obtained were dried under reduced pressure at 50° C. for 14 hours and 35 minutes to obtain the title compound (152 g).

Provenance & Evidence