Hydrochloric Acid → 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride

HRID 2263262노트

반응식

HRID 2263262 반응식
[ClH:1].[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][CH2:16]2)[S:13][CH:14]=1.CCCCCC>C(OCC)(=O)C>[ClH:1].[F:2][C:3]1[C:8]([F:9])=[CH:7][CH:6]=[CH:5][C:4]=1[C:10]1[N:11]=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[S:13][CH:14]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 68781293Tert-butyl 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate

생성물 1

HCID 687762881-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A 4 N solution (50 ml) of hydrogen chloride in ethyl acetate was added to a solution of tert-butyl 4-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine-1-carboxylate (4.20 g, 11.0 mmol) in ethyl acetate (100 ml), and the mixture was stirred at room temperature for 14 hours. Hexane was added to the reaction mixture, and crystals were collected by filtration to give 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride. The hydrochloride was dissolved in water, neutralized with a 1 N sodium hydroxide aqueous solution, and extracted with chloroform. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give 1.76 g (56.8%) of the desired product as a solid.

후처리

  1. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-dc32fcfb544e4a39b5e700b7d2f522cf
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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