300543-56-0, (R)-1-((4-Chlorophenyl)(phenyl)methyl)piperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
40.0 g of 1-[(R)-(4-chlorophenyl) (phenyl) methyl] piperazine, 14.1 g of sodium hydrogen carbonateAnd a mixture of 78.1 g of N-methyl-2-pyrrolidoneHeat to 120 C, ethyl (2-chloroethoxy) acetateAfter 27.9 g was dropped over 30 minutes, the mixture was stirred for 6 hours.After cooling the obtained suspension to room temperature, 200 g of waterAnd toluene 69gAnd the mixture was separated.120 g of water is added to the obtained organic layer, and liquid separation is performed again to obtain the formula (6).; Example 1 32 g of water was added to a toluene solution of the compound (6) obtained in Reference Example 1, and a solution of 7.0 g of lithium hydroxide monohydrate dissolved in 44 g of water was added dropwise at room temperature. It stirred until it became 0.2% or less. Liquid separation was carried out after the obtained solution, 8 g of N-methyl-2-pyrrolidone for washing, 139 g of toluene and 25 g of acetone were mixed. To the separated aqueous layer were added 139 g of toluene and 13 g of acetone to carry out liquid separation again. Further, 139 g of toluene and 9 g of acetone were added to the separated aqueous layer, and liquid separation was performed again. 35 g of toluene and 193 g of methyl ethyl ketone were added to the obtained aqueous layer, and 29.1 g of 35% hydrochloric acid was dropped to adjust the pH to 2.4, and the solution was heated to 45 C. to separate. After 35 g of toluene was added to the obtained organic layer, concentration was performed until the remaining amount became 95 g. Furthermore, 97 g of methyl ethyl ketone and 35 g of toluene were added and concentrated until the remaining amount reached 99 g, and further 24 g of methyl ethyl ketone and 9 g of toluene were added and concentrated until the remaining amount became 101 g. After adding methyl ethyl ketone 64g and acetone 411g at room temperature and dropping 7.3g of 35% hydrochloric acid,0.04 g of levocetirizine dihydrochloride was added.Subsequently, 316 g of acetone was dropped, and after stirring for 1.5 hours, 6.9 g of 35% hydrochloric acid was dropped. After filtering the obtained suspension, the obtained solid was washed with 95 g of acetone. The obtained crystals were dried under reduced pressure at 40 C. to obtain 54.6 g of levocetirizine dihydrochloride. The purity was 99.8% or more, 300543-56-0
The synthetic route of 300543-56-0 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; Sumitomo Chemical Co., Ltd.; Yoshida, Kazuhiro; Ando, Kenichi; (13 pag.)JP2019/43885; (2019); A;,
Piperazine – Wikipedia
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