Hydrochloric Acid → HCID 178488693, compound

Participants

Reaction Conditions

Reaction Steps

Under argon gas atmosphere, to a solution of the compound prepared in Example 1 (38.7 g) in toluene, acetic acid (14.5 mL) and 60% aqueous solution of hydrazine hydrate (17.7 mL) were sequentially added at 10 to 30° C. of internal temperature. The mixture was stirred for 7 hours at 45 to 55° C. of internal temperature. To the reaction solution cooled to 10 to 30° C. of internal temperature, 2 mol/L hydrochloric acid was added and then the mixture was separated. The aqueous layer was adjusted to pH 6.5 to 7.5 by adding 25 wt % sodium hydroxide. Isopropyl acetate (216 mL) was added to the adjusted aqueous layer. The separated organic layer was concentrated under reduced pressure. The residue was heated, and n-heptane was added. The solution was cooled to 10 to 30° C. of internal temperature. After the crystal was precipitated, the solution was stirred for 30 minutes. Furthermore, n-heptane was added to the solution, and the mixture was stirred for 1 hour. The precipitated crystal was collected by filtration, dried under reduced pressure for 14 hours or more at about 50° C. to give the title compound having the following physical data (35.5 g (94.8 area %); quantitative value: 61% (2 processes)).

Provenance & Evidence