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Hydrazine hydrate (1:1) → (S)-5-(aminomethyl)-3-(3-fluoro-4-iodophenyl)oxazolidin-2-one

HRID 1949192
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1949192
[F:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][C@@H:12]([CH2:14][N:15]3C(=O)C4C(=CC=CC=4)C3=O)[O:11][C:10]2=[O:26])[CH:5]=[CH:6][C:7]=1[I:8].O.NN>C(O)C>[NH2:15][CH2:14][C@@H:12]1[O:11][C:10](=[O:26])[N:9]([C:4]2[CH:5]=[CH:6][C:7]([I:8])=[C:2]([F:1])[CH:3]=2)[CH2:13]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 66884332(5R)-2-[3-(3-fluoro-4-iodo-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-isoindole-1,3-dione

Produkt 1

HCID 58721926(S)-5-(aminomethyl)-3-(3-fluoro-4-iodophenyl)oxazolidin-2-oneAusbeute 95,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of (5R)-2-[3-(3-fluoro-4-iodo-phenyl)-2-oxo-oxazolidin-5-ylmethyl]-isoindole-1,3-dione (1021, 23.3 g, 50.0 mmol) in ethanol (EtOH, 150 mL) was treated with hydrazine monohydrate (12.52 g, 12.1 mL, 250 mmol, 5.0 equiv) at 25° C., and the resulting reaction mixture was warmed up to reflux for 2 h. White precipitates were formed while the reaction mixture was refluxed. When TLC and HPLC showed that the reaction was complete, the reaction mixture was cooled down to room temperature before being quenched with H2O (100 mL). The white precipitates were totally dissolved when water was introduced into the reaction mixture and a homogeneous solution was generated. The aqueous solution was then extracted with CH2Cl2 (3×200 mL), and the combined organic extracts were washed with H2O (2×100 mL) and saturated NaCl aqueous solution (100 mL), dried over MgSO4, and concentrated in vacuo. The residue was further dried in vacuo to afford the crude (5S)-5-aminomethyl-3-(3-fluoro-4-iodo-phenyl)-oxazolidin-2-one (1022, 16.0 g, 16.8 g theoretical, 95.2%) as white powders, which were found to be essentially pure and was directly used in the subsequent reactions without further purifications. For 1022: C10H10FIN2O2, LCMS (EI) m/e 337 (M++H).

Aufarbeitung

  1. customthe resulting reaction mixture
  2. temperaturewas warmed up
  3. temperatureto reflux for 2 h
  4. customWhite precipitates
  5. customwere formed while the reaction mixture
  6. temperaturewas refluxed
  7. custombefore being quenched with H2O (100 mL)
  8. customThe white precipitates
  9. dissolutionwere totally dissolved when water
  10. additionwas introduced into the reaction mixture
  11. extractionThe aqueous solution was then extracted with CH2Cl2 (3×200 mL)
  12. washthe combined organic extracts were washed with H2O (2×100 mL) and saturated NaCl aqueous solution (100 mL)
  13. dry with materialdried over MgSO4
  14. concentrationconcentrated in vacuo
  15. customThe residue was further dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-cb71d80201f640fa8f9891483b3447ca
Quelldatensatz
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08399660B2

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