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

HRID 730749ノート

反応式

HRID 730749 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-af55003f34a642b7875330fd478a5792
出典データセット
uspto-grants-2009_09
特許番号
US07582761B2

反応ノート

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