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

HRID 1047370
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HRID 1047370 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-70fcfa7cb4ca41dc8e6985d4696de469
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08569495B2

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