Reaktion #84375

ord-99e1f1d0b8b147e5b818e5bd1574fa0a

Reaktionsgleichung

O=C([O-])[O-].[K+].[K+]
K2CO3
Cl.O=S1(=O)CCNCC1
1,1-dioxo-thio-morpholinehydrochloride
O=[N+]([O-])c1ccc(F)c(F)c1
3,4-difluoronitrobenzene
O=[N+]([O-])c1ccc(N2CCS(=O)(=O)CC2)c(F)c1
title compound
Ausbeute 110.1%
O=[N+]([O-])c1ccc(N2CCS(=O)(=O)CC2)c(F)c1
4-(2-fluoro-4-nitrophenyl)1,1-dioxidothiomorpholine
Ausbeute 110.1%

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with CH2Cl2 (100 mL×2)
  2. 2
    TrocknenThe combined organic phases were dried over anhydrous Na2SO4
  3. 3
    Einengenconcentrated in vacuo

Vorschrift

To a suspension of K2CO3 (5.53 g, 40 mmol) and 1,1-dioxo-thio-morpholinehydrochloride (3.60 g, 21 mmol) in DMSO (50 mL) was added 3,4-difluoronitrobenzene (3.18 g, 20 mmol). The reaction was heated at 100° C. for 12 h. The mixture was diluted with water (150 mL) and extracted with CH2Cl2 (100 mL×2). The combined organic phases were dried over anhydrous Na2SO4 and concentrated in vacuo to give the title compound as a yellow solid (6.04 g, 70%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09434695B2uspto-grants-2016_09