Sodium Hydroxide → 1-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine

HRID 2263263

반응식

HRID 2263263 반응식
Cl.[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.[OH-].[Na+]>O>[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

4

반응물 2

HCID 14798Sodium HydroxideHCID 687762881-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine hydrochloride

생성물 1

HCID 687762891-[4-(2,3-Difluorophenyl)-1,3-thiazol-2-yl]piperazine수율 56.8%

시약·촉매·용매 1

HCID 962Water용매

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. extractionextracted with chloroform
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-a0dc484bb6a1418eaf18f6d2c2bc8459
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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