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1-Boc-4-(3-(ethoxycarbonyl)phenyl)piperazine → 3-(4-(Tert-butoxycarbonyl)piperazin-1-yl)benzoic acid

HRID 2047367
ノート
印刷プレビュー

反応式

HRID 2047367 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([O:22]CC)=[O:21])[CH:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CCO.[OH-].[Na+]>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([OH:22])=[O:21])[CH:15]=2)[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 162179411-Boc-4-(3-(ethoxycarbonyl)phenyl)piperazine

生成物 1

HCID 448287263-(4-(Tert-butoxycarbonyl)piperazin-1-yl)benzoic acid収率 85.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 4-(3-ethoxycarbonyl-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (5.00 g, 14.95 mmol) in EtOH (50 mL) and NaOH 10% (20 mL) was refluxed for 3 h, then the reaction mixture was cooled to room temperature and the organic solvent evaporated under reduced pressure. The resulting solution was neutralized by the dropwise addition of 1N HCl and the aqueous solution was extracted with EtOAc (3×50 mL) The combined organic layers were dried over Na2SO4, filtered, and concentrated under reduced pressure to obtain 3.90 g of the title compound (85%) without further purification.

後処理

  1. customthe organic solvent evaporated under reduced pressure
  2. additionThe resulting solution was neutralized by the dropwise addition of 1N HCl
  3. extractionthe aqueous solution was extracted with EtOAc (3×50 mL) The combined organic layers
  4. dry with materialwere dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-93898ce3a10a4e90865a4477ab808f3b
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592463B2

反応ノート

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