Win 35428 → 53898-64-9

HRID 1453980

Reaktionsgleichung

Reaktionsgleichung von HRID 1453980
[C:1]([C@H:5]1[C@@H:11]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:10][C@H:9]2[N:19]([CH3:20])[C@@H:6]1[CH2:7][CH2:8]2)([O:3]C)=[O:2]>O1CCOCC1.O>[C:1]([C@H:5]1[C@@H:11]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)[CH2:10][C@H:9]2[N:19]([CH3:20])[C@@H:6]1[CH2:7][CH2:8]2)([OH:3])=[O:2]

Komponenten

3

Edukt 1

HCID 105056Win 35428

Produkt 1

HCID 1086911253898-64-9

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 218864351,4-Dioxane--water (1/1)Lösungsmittel

Versuchsvorschrift

2β-Carbomethoxy-3β-(4-fluorophenyl)tropane (WIN 35,428) (1), is boiled for 24 h in a 1:1 dioxane-water solution. The solvent is removed in vacuo and the residue is almost completely dissolved in CHCl3. Remaining undissolved solid can then be filtered off, toluene can then be added, and the volume of the solution is reduced in vacuo to approximately 25%. Cooling the resulting white suspension in a freezer for 2 h will provide a precipitated solid which can then be isolated by filtration and is washed with cold 1:1 CHCl3-toluene. The solid can then be pumped dry to give the product.

Aufarbeitung

  1. customThe solvent is removed in vacuo
  2. dissolutionthe residue is almost completely dissolved in CHCl3
  3. filtrationcan then be filtered off
  4. additiontoluene can then be added
  5. temperatureCooling the resulting white suspension in a freezer for 2 h
  6. customwill provide a precipitated solid which
  7. customcan then be isolated by filtration
  8. washis washed with cold 1:1 CHCl3-toluene
  9. customThe solid can then be pumped dry
  10. customto give the product

Quellen und Nachweise

ORD-Eintrag
ord-3550ea0a7d1f4d248e4c52837af96eb5
Quelldatensatz
uspto-grants-2009_01
Patentnummer
US07476740B2

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