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2-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide → 2-((S)-3-hydroxy-1,1-dimethyl-3-trifluoromethylhex-5-ynyl)benzamide

HRID 2387328
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2387328
[OH:1][C@@:2]([C:23]([F:26])([F:25])[F:24])([CH2:16][C:17]#[C:18][Si](C)(C)C)[CH2:3][C:4]([C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9]([NH2:11])=[O:10])([CH3:6])[CH3:5]>C1COCC1>[OH:1][C@@:2]([C:23]([F:24])([F:25])[F:26])([CH2:16][C:17]#[CH:18])[CH2:3][C:4]([C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9]([NH2:11])=[O:10])([CH3:5])[CH3:6]
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Komponenten

3

Edukt 1

HCID 580261722-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide

Produkt 1

HCID 580261202-((S)-3-hydroxy-1,1-dimethyl-3-trifluoromethylhex-5-ynyl)benzamideAusbeute 69,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a stirred, ice-cooled, THF solution (100 mL) of 2-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide (17.8 g, 46.2 mmol) n-tetrabutylammonium fluoride was added (51 mL of 1 M solution in THF, 51 mmol) dropwise via addition funnel. After 30 minutes, the reaction was quenched with 200 mL of 1 M HCl and further diluted with brine. The mixture was extracted with ethyl acetate. The combined extract was washed with water and brine, dried over anhydrous sodium sulfate, and the solvent removed in vacuo. The residue was redissolved in dichloromethane and the solvent evaporated. The residue was then dissolved in 30 mL of diethyl ether and triturated with hexanes. The precipitated solid was filtered. The filtrate was collected and the solvent evaporated, and the residue treated with diethyl ether/hexanes as before to obtain more solid precipitate. The solids were combined and dried in vacuo to give 2-((S)-3-hydroxy-1,1-dimethyl-3-trifluoromethylhex-5-ynyl)benzamide (10 g, 33% over two steps). This material was used without further purification.

Aufarbeitung

  1. temperatureTo a stirred, ice-cooled
  2. additiondropwise via addition funnel
  3. customthe reaction was quenched with 200 mL of 1 M HCl
  4. additionfurther diluted with brine
  5. extractionThe mixture was extracted with ethyl acetate
  6. extractionThe combined extract
  7. washwas washed with water and brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. customthe solvent removed in vacuo
  10. dissolutionThe residue was redissolved in dichloromethane
  11. customthe solvent evaporated
  12. dissolutionThe residue was then dissolved in 30 mL of diethyl ether
  13. customtriturated with hexanes
  14. filtrationThe precipitated solid was filtered
  15. customThe filtrate was collected
  16. customthe solvent evaporated
  17. additionthe residue treated with diethyl ether/hexanes as before
  18. customto obtain more solid precipitate
  19. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-45f173db075745ff901c5ff22fc80ca1
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08268859B2

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