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Sodium hydride → 1-(4-(4-Trifluoromethyl-benzyloxy)-phenyl)-piperazine

HRID 1047370
ノート
印刷プレビュー

反応式

HRID 1047370 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11](C(O)=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[H-].[Na+].Br[CH2:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=1>O1CCCC1>[F:28][C:27]([F:29])([F:30])[C:24]1[CH:25]=[CH:26][C:21]([CH2:20][O:1][C:2]2[CH:3]=[CH:4][C:5]([N:8]3[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]3)=[CH:6][CH:7]=2)=[CH:22][CH:23]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 1230621-(Bromomethyl)-4-(trifluoromethyl)benzeneHCID 220369224-(4-Hydroxy-phenyl)-piperazine-1-carboxylic acid

生成物 1

HCID 585767301-(4-(4-Trifluoromethyl-benzyloxy)-phenyl)-piperazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

A solution of 4-(4-hydroxy-phenyl)-piperazine-1-carboxylic acid tent-butyl ester (1.5 g, 5.4 mmol) in dry tetrahydrofuran (5 mL) was added to a suspension of sodium hydride (431 mg, 60% in oil, 10.8 mmol) in dry tetrahydrofuran (35 mL). After 15 min, a solution of 1-bromomethyl-4-trifluoromethyl-benzene (1.9 g, 8.1 mmol) in tetrahydrofuran (5 mL) was added. The mixture was stirred for 16 hr at room temperature, filtered, and concentrated under vacuum. The resulting residue was diluted in ethyl acetate (40 mL), and the organic layer was washed with water (3×20 mL), dried over magnesium sulfate, filtered, and concentrated under vacuum. The resulting residue was dissolved in a 1:1 mixture of dichloromethane and trifluoroacetic acid (30 mL). The mixture was then stirred for 30 min. Afterward, the mixture was concentrated under vacuum, taken up in dichloromethane (30 mL), and evaporated to dryness. The resulting residue was diluted in diethylether (5 mL) and then combined with a molar solution of HCl in diethylether (10 mL, 1M). A precipitate formed, which was filtered, washed with diethylether (10 mL), and dried under vacuum. The desired product was isolated as a hydrochloride salt with traces of solvent.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated under vacuum
  3. additionThe resulting residue was diluted in ethyl acetate (40 mL)
  4. washthe organic layer was washed with water (3×20 mL)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. dissolutionThe resulting residue was dissolved in a 1:1 mixture of dichloromethane and trifluoroacetic acid (30 mL)
  9. stirringThe mixture was then stirred for 30 min
  10. concentrationAfterward, the mixture was concentrated under vacuum
  11. customevaporated to dryness
  12. additionThe resulting residue was diluted in diethylether (5 mL)
  13. customA precipitate formed
  14. filtrationwhich was filtered
  15. washwashed with diethylether (10 mL)
  16. customdried under vacuum

出典と根拠

ORDレコード
ord-70fcfa7cb4ca41dc8e6985d4696de469
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569495B2

反応ノート

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