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Hydrochloric Acid → (R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-

HRID 1500200
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1500200
CC1(C)[O:6][C@@H:5]([C:7]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]3[CH:20]=[CH:19][C:18]([O:21][C:22]4[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=4)=[CH:17][CH:16]=3)[N:10]=2)=[O:8])[CH2:4][O:3]1.C(Cl)Cl.CO.Cl.O>O1CCOCC1.C(Cl)Cl.C([O-])(O)=O.[Na+]>[F:28][C:25]1[CH:24]=[CH:23][C:22]([O:21][C:18]2[CH:19]=[CH:20][C:15]([C:11]3[N:10]=[C:9]([C:7](=[O:8])[C@H:5]([OH:6])[CH2:4][OH:3])[CH:14]=[CH:13][CH:12]=3)=[CH:16][CH:17]=2)=[CH:27][CH:26]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 21226129Dichloromethane methanolHCID 89822495(R)-(2,2-dimethyl-1,3-dioxolan-4-yl)(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)methanone

Produkt 1

HCID 71722102(R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-Ausbeute 28 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6344DichloromethaneLösungsmittelHCID 312751,4-DioxaneLösungsmittelHCID 516892Sodium BicarbonateLösungsmittel

Versuchsvorschrift

To a solution of (R)-(2,2-dimethyl-1,3-dioxolan-4-yl)(6-(4-(4-fluorophenoxyl)phenyl)pyridin-2-yl)methanone (0.621, g, 1.58, mmol) in an 85:15, mixture of DCM/MeOH (10, mL) was added 4M HCl in dioxane (2, mL, 8, mmol). After stirring overnight 0.5, mL, water was added to the reaction. After 3, more hours the reaction was diluted with 50, mL DCM and solid NaHCO3, was added. After the bubbling subsided, the reaction mixture was dried over Na2SO4, filtered, and evaporated in vacuo to a residue. The residue was chromatographed over silica gel with 10-75% acetone in hexanes. The product fractions were isolated and evaporated in vacuo. The residue was dissolved in acetone, evaporated in vacuo, dissolved in EtOAc and hexanes, evaporated in vacuo, treated with hexanes, and evaporated in vacuo. The material was dried under vacuum at 50° C. to give the product (R)-1-(6-(4-(4-fluorophenoxy)phenyl)pyridin-2-yl)-2,3-dihydroxypropan-1-one as a glassy orange solid (0.155, g, 0.44, mmol, 28% yield). LC/MS: m/z=354.1, [M+H]+, ; 1H NMR (400, MHz, DMSO-d6): 8.23-8.17, (3 H, m), 8.08, (1 H, t, J=7.9, Hz), 7.88, (1 H, dd, J=7.7, Hz, 0.9, Hz), 7.32-7.25, (2 H, m), 7.20-7.15, (2 H, m), 7.12, (2 H, d, J=9.0, Hz), 5.54-5.49, (1 H, m), 5.09, (1 H, d, J=7.0, Hz), 4.78, (1 H, t, J=5.5, Hz), 3.93-3.81, (2 H, m). Unless otherwise indicated all 1H NMR chemical shifts reported herein are denoted by the delta (δ) scale.

Aufarbeitung

  1. additionwas added
  2. dry with materialthe reaction mixture was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated in vacuo to a residue
  5. customThe residue was chromatographed over silica gel with 10-75% acetone in hexanes
  6. customThe product fractions were isolated
  7. customevaporated in vacuo
  8. dissolutionThe residue was dissolved in acetone
  9. customevaporated in vacuo
  10. dissolutiondissolved in EtOAc
  11. customhexanes, evaporated in vacuo
  12. additiontreated with hexanes
  13. customevaporated in vacuo
  14. customThe material was dried under vacuum at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-a49d85b2d3f143c884ef14301c155784
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09206127B2

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