Perboric acid, sodium salt, monohydrate → HCID 68815368, Verbindung

HRID 732436Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 732436
B(O[O-])=O.[OH2:5].[Na+].[CH3:7][O:8][C:9](=[O:25])[C:10]1[CH:15]=[C:14]([S:16][CH2:17][CH2:18][CH3:19])[N:13]=[C:12]([NH:20][C@H:21]([CH2:23][CH3:24])[CH3:22])[CH:11]=1>C(O)(=O)C>[CH3:7][O:8][C:9](=[O:25])[C:10]1[CH:15]=[C:14]([S@:16]([CH2:17][CH2:18][CH3:19])=[O:5])[N:13]=[C:12]([NH:20][CH:21]([CH2:23][CH3:24])[CH3:22])[CH:11]=1

Komponenten

4

Edukt 2

HCID 23695970Perboric acid, sodium salt, monohydrateHCID 68814642HCID 68814642, Verbindung

Produkt 1

HCID 68815368HCID 68815368, VerbindungAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Add sodium perborate monohydrate (0.133 g, 1.33 mmol) to a cooled solution of (S)-2-sec-butylamino-6-propylsulfanyl-isonicotinic acid methyl ester (0.396 g, 1.40 mmol) in acetic acid (4 mL). Stir at room temperature overnight and concentrate. Dissolve the residue in ethyl acetate and wash the solution with aqueous sodium bicarbonate, saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes) to give the title compound (0.230 g, 55%).

Aufarbeitung

  1. concentrationconcentrate
  2. dissolutionDissolve the residue in ethyl acetate
  3. washwash the solution with aqueous sodium bicarbonate, saturated aqueous sodium chloride
  4. dry with materialdry (magnesium sulfate)
  5. concentrationconcentrate
  6. custompurify
  7. wash(silica gel chromatography, eluting with 30:70 ethyl acetate:hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-9e4ac74249144bb488860c078f4a9688
Quelldatensatz
uspto-grants-2009_09
Patentnummer
US07585885B2

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