Carbon Dioxide → HCID 67457963, compound

Participants

Reaction Conditions

Reaction Steps

Under the protection of N2, 1-((1S)-5-bromo-2,3-dihydro-1H-inden-1-yl)-4-methylpiperazine (660 g, 2.235 mol) and THF (3.3 L) were added to a 10 L three-neck flask, and the solution was stirred until dissolved. The system temperature was cooled to −78° C. in liquid nitrogen-acetone bath. n-butyllithium (n-BuLi) (2.5 M in hexane solution) (1072 mL, 2.682 mol, 1.2-fold) was added dropwise into the solution at −78° C.˜−82° C. After being stirred for 10 minutes, when the LC-MS assay shown that the reaction of the raw materials was completed, dry ice (170 g, 3.86 mol, 1.73-fold) was added carefully. The solution was then stirred for 10 minutes at −60° C.˜−75° C. After the reaction was completed, the cold bath was removed and aqueous solution of 2 N HCl was then added to adjust the pH value till pH=2. Most of the water was removed using rotary evaporator. The system was further dried overnight at 50° C.˜60° C. in a vacuum drying oven to obtain the title compound (1289 g, the actual product of 583 g providing 100% yield). This crude product was used in the next step of reaction directly.

Provenance & Evidence