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Water → 4-Nitrophenyl thiomorpholine-4-carboxylate 1-oxide

HRID 661213
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 661213
[N:1]1([C:7]([O:9][C:10]2[CH:15]=[CH:14][C:13]([N+:16]([O-:18])=[O:17])=[CH:12][CH:11]=2)=[O:8])[CH2:6][CH2:5][S:4][CH2:3][CH2:2]1.ClC1C=CC=C(C(OO)=[O:27])C=1.O>ClCCl>[N:1]1([C:7]([O:9][C:10]2[CH:11]=[CH:12][C:13]([N+:16]([O-:18])=[O:17])=[CH:14][CH:15]=2)=[O:8])[CH2:2][CH2:3][S:4](=[O:27])[CH2:5][CH2:6]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 581164954-Nitrophenyl thiomorpholine-4-carboxylate

Produkt 1

HCID 581165434-Nitrophenyl thiomorpholine-4-carboxylate 1-oxide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

13.1 g (49.0 mmol) of 4-nitrophenyl thiomorpholine-4-carboxylate were initially charged in 135 ml of dichloromethane and admixed at 0° C. with 7.6 g (44.1 mmol) of m-chloroperbenzoic acid in portions. The mixture was stirred at RT for two hours, water was added and the organic phase was removed. The organic phase was washed rapidly with saturated aqueous sodium hydrogencarbonate solution, filtered and concentrated under reduced pressure. The crude product was purified by means of preparative HPLC. Yield: 7.8 g (56% of theory)

Aufarbeitung

  1. customthe organic phase was removed
  2. washThe organic phase was washed rapidly with saturated aqueous sodium hydrogencarbonate solution
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by means of preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-67247df07d3f4f4fa6aff63b997bee3e
Quelldatensatz
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08084469B2

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