Hydrochloric Acid → 1-(3,5-Difluoropyridin-2-yl)piperazine

HRID 730749노트

반응식

HRID 730749 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:19]([F:20])=[CH:18][C:17]([F:21])=[CH:16][N:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>O1CCOCC1>[F:20][C:19]1[C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[N:15][CH:16]=[C:17]([F:21])[CH:18]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 674014754-(3,5-Difluoro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 451164141-(3,5-Difluoropyridin-2-yl)piperazine

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 4-(3,5-difluoro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester from step (b) above (140 mg, 0.47 mmol) and 4 M solution of HCl in dioxane (1 mL, Aldrich) was stirred at room temperature for 30 h. The solvent was evaporated in vacuo and the residue was dissolved in EtOAc (30 mL). The solution was washed successively with 1 N NaOH (20 mL) and brine (20 mL), dried over MgSO4, filtered, and the solvent was removed in vacuo. The residue was purified by silica gel chromatography, eluting with 10% MeOH in CH2Cl2 to give the title compound as a white solid. MS (ESI, pos. ion) m/z: 200 (M+1).

후처리

  1. customThe solvent was evaporated in vacuo
  2. dissolutionthe residue was dissolved in EtOAc (30 mL)
  3. washThe solution was washed successively with 1 N NaOH (20 mL) and brine (20 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo
  7. customThe residue was purified by silica gel chromatography
  8. washeluting with 10% MeOH in CH2Cl2

출처 및 근거

ORD 기록
ord-af55003f34a642b7875330fd478a5792
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07582761B2

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